A supergravity distillation device and a supergravity distillation method for catalytically removing solid from oil slurry

Abstract

The application provides a supergravity distillation device and a desolidification distillation method for catalytic oil slurry, and the supergravity distillation device comprises a feeding section, a stripping section and a supergravity rectification section arranged in sequence; the supergravity rectification section is provided with a rotating shaft, at least three rotors are arranged on the rotating shaft from top to bottom, a sleeve pipe is arranged along the rotating shaft as a liquid collecting groove, and the outer ring of the sleeve pipe is provided with a filler. The supergravity distillation device can sufficiently remove the ash in the catalytic oil slurry, so that the catalytic oil slurry can be used to produce high-quality needle coke raw materials; the supergravity distillation device can simultaneously realize the fraction cutting of the catalytic oil slurry without filtering, reduces the equipment investment and the operation cost, and has a good application prospect and economic benefits.

Description

Technical Field

[0001] This invention belongs to the field of petrochemical technology and relates to a high-gravity distillation apparatus and a distillation method for catalytic oil slurry desolidification. Background Technology

[0002] Needle coke possesses a series of advantages, including a low coefficient of thermal expansion, low porosity, low sulfur content, low ash content, low metal content, high electrical conductivity, and ease of graphitization. Its graphitized products exhibit good chemical stability, corrosion resistance, high thermal conductivity, good mechanical strength at both low and high temperatures, and excellent overall electrochemical performance. These superior properties make it a high-quality raw material for manufacturing ultra-high-power graphite electrodes and lithium-ion battery anode materials. The nation's continued promotion of industrial restructuring and transformation in the steel and automotive industries, along with the vigorous advancement of energy-saving, low-carbon, and green technologies, has spurred the rapid development of electric arc furnace steelmaking and new energy vehicles, leading to a significant increase in demand for needle coke.

[0003] Catalytic oil slurry contains a large number of impurities, such as gums, asphaltenes, sulfur and nitrogen, and catalyst powder. The presence of these impurities seriously affects the quality of needle coke. Producing high-end needle coke requires the ash content of the catalytic oil slurry to be below 100 ppm. Existing methods for removing ash from the slurry include filtration, vacuum distillation, and solvent extraction. Commonly used filtration processes include sedimentation, centrifugation, mechanical filtration, and ceramic membrane filtration, with mechanical filtration and ceramic membrane filtration being the most widely applied. Mechanical filtration uses sintered metal filter elements as the filter medium, but suffers from short operating cycles, frequent filtration mode switching, and easy clogging of the filter elements. Membrane filtration uses ceramic membranes as the filter medium, which requires regular cleaning and has high operating costs. Vacuum distillation can remove catalytic oil slurry powder, but the removal rate is limited and difficult to meet the requirements for needle coke feedstock. Solvent extraction can effectively remove catalytic oil slurry powder, but the investment cost is high.

[0004] CN 111534322B developed a purification device for producing needle coke feedstock. By adjusting the backflushing pressure of the filter according to the filter pressure difference and the number of backflushing cycles during the initial and middle stages of filter operation, a permanent filter cake is established to prevent particulate matter from entering the filter element, thus achieving long-term stable operation of the filtration equipment.

[0005] CN113862035A describes a process where catalytic oil slurry is filtered, and the filtered liquid product is subjected to vacuum distillation. The intermediate fraction obtained from vacuum distillation is hydrogenated to remove impurities such as sulfur and nitrogen. This hydrogenated oil is then coked to produce needle coke. The bottom slurry residue from vacuum distillation is blended and sold as road asphalt.

[0006] The above patents employ a combination of filtration and vacuum distillation to remove impurities such as ash and asphalt during the pretreatment of catalytic oil slurry. The oil slurry yield after filtration is around 80-90%, but the investment and operating costs of the two sets of equipment are relatively high.

[0007] Therefore, providing a high-gravity distillation apparatus and method for desolidation of catalytic oil slurry, improving the distillation and desolidation efficiency of catalytic oil slurry, and reducing equipment investment is of great significance for improving the economic benefits of needle coke enterprises. Summary of the Invention

[0008] To address the problems existing in the prior art, this invention provides a supergravity distillation apparatus and method for deconsolidating catalytic oil slurry. The supergravity distillation apparatus can effectively remove ash from the catalytic oil slurry, making it usable for producing high-quality needle coke feedstock. The supergravity distillation apparatus eliminates the need for filtration and simultaneously achieves fractionation of the catalytic oil slurry, reducing equipment investment and operating costs, and has good application prospects and economic benefits.

[0009] To achieve the above-mentioned technical effects, the present invention adopts the following technical solution:

[0010] One objective of this invention is to provide a high-gravity distillation apparatus for catalytic desolidification of oil slurry, the high-gravity distillation apparatus comprising a feed section, a stripping section, and a high-gravity rectification section arranged sequentially.

[0011] The supergravity distillation section is equipped with a rotating shaft connected to an electric drive device. The rotating shaft has at least three rotors arranged from top to bottom. Each rotor has a first gas outlet above its connection with the rotating shaft. A sleeve is arranged along the rotating shaft as a liquid collection tank. Holes are distributed around the sleeve, and packing is arranged around the outer ring of the sleeve. A second gas outlet is arranged in the cavity formed by the first gas outlet and the tower body. The second gas outlet is connected to a condensing device, and the condensate outlet of the condensing device is connected to the liquid collection tank.

[0012] The number of rotors can be 3, 4, 5, 6, 7, 8, 9 or 10, but is not limited to the listed values. The number of rotors can be adjusted according to properties such as the ash content in the catalytic slurry.

[0013] In this invention, under hypergravity, the liquid is stretched into micron and nanometer-sized droplets and filaments, creating a huge and rapidly renewing phase interface. This increases the gas-liquid contact area, enhances mass and heat transfer, and improves the distillation efficiency of the catalytic oil slurry. The catalyst powder contained in the catalytic oil slurry is encapsulated and separated by the droplets under hypergravity, enabling effective ash removal. The intermediate fraction of the catalytic oil slurry can serve as a high-quality raw material for needle coke.

[0014] In this invention, the gas flowing out of the gas outlet of the next rotor layer comes into full contact with the liquid in the cavity and then flows out through the gas outlet of the previous rotor layer before entering the cavity of the next rotor layer.

[0015] As a preferred embodiment of the present invention, the stripping section is provided with at least two layers of herringbone trays arranged alternately. The number of herringbone trays can be 2, 5, 10, 15, 20, 25, or 30 layers, etc., but is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0016] As a preferred embodiment of the present invention, the feeding section is provided with a catalytic oil slurry inlet and a quench oil inlet.

[0017] Preferably, the catalytic oil slurry inlet is connected to a catalytic oil slurry distribution device.

[0018] Preferably, the quench oil inlet is connected to a quench oil distribution device.

[0019] Preferably, the nozzle of the quench oil distribution device is inclined downwards towards the bottom of the tower at an angle of 30 to 60°, such as 30°, 35°, 40°, 45°, 50°, 55° or 60°, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0020] As a preferred embodiment of the present invention, the supergravity distillation apparatus further includes a vacuum pumping component.

[0021] As a preferred technical solution of the present invention, the bottom of the supergravity distillation apparatus is provided with an anti-coking component.

[0022] Preferably, the bottom of the supergravity distillation apparatus is provided with an oil outlet, and the oil outlet is provided with a coke filter.

[0023] In this invention, a coke filter is installed at the bottom of the supergravity distillation apparatus to block coke and prevent the oil outlet pipeline at the bottom of the tower from becoming clogged.

[0024] In this invention, the liquid collection tank can be annular with small holes evenly distributed around its perimeter.

[0025] In this invention, the pore size of the filler can be 30-50 μm, such as 30 μm, 32 μm, 35 μm, 38 μm, 40 μm, 42 μm, 45 μm, 48 μm or 50 μm, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0026] The second objective of this invention is to provide a catalytic oil slurry deconsolidation distillation method, wherein the deconsolidation distillation method uses the high-gravity distillation apparatus for catalytic oil slurry deconsolidation provided in the first objective, and the catalytic oil slurry deconsolidation distillation method includes:

[0027] The catalytic slurry enters the supergravity distillation unit via the feed section, and after being vaporized in the stripping section, it enters the supergravity rectification section.

[0028] As the vaporized catalytic slurry moves upward, it sequentially contacts the droplets generated by each rotor to form a gas-liquid mixture.

[0029] The catalyst powder in the gas-liquid mixture is thrown towards the cavity formed by the first gas outlet and the tower body under the action of gravity, and enters the liquid collection tank with the liquid.

[0030] In this invention, the gasified catalytic slurry comes into full contact with the droplets coming out of the rotor for mass and heat transfer. The catalyst powder carried in the gas and liquid is thrown into the cavity under the action of gravity and flows into the collection tank with the liquid. After being washed by at least 3 rotors, the solid particles of catalyst in the catalytic slurry distillate can be effectively removed. The middle distillate of the catalytic slurry can be used as a high-quality raw material for needle coke.

[0031] As a preferred technical solution of the present invention, the feed temperature of the catalytic slurry is 350-370℃, such as 350℃, 352℃, 355℃, 358℃, 360℃, 362℃, 365℃, 368℃ or 370℃, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0032] As a preferred technical solution of the present invention, quenching oil is used to reduce the temperature at the bottom of the supergravity distillation apparatus.

[0033] In this invention, the bottom temperature of the supergravity distillation apparatus is high and contains a large amount of catalyst powder. To prevent coking, a low-temperature catalytic oil slurry is promptly injected through a quench oil distributor. The slurry is quickly and thoroughly mixed with the heavy fraction of the bottom oil slurry through the distributor. Since the nozzle is tilted downwards, it can enhance the turbulence of the liquid at the bottom of the column and reduce the temperature at the bottom of the column in a timely manner.

[0034] Preferably, the quenching oil is a catalytic slurry with a temperature of 100-150°C, such as 100°C, 110°C, 120°C, 130°C, 140°C, or 150°C, but it is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0035] As a preferred technical solution of the present invention, the rotational speed of the rotor is 800 to 3000 rpm, such as 800 rpm, 1000 rpm, 1200 rpm, 1500 rpm, 1800 rpm, 2000 rpm, 2200 rpm, 2500 rpm, 2800 rpm or 3000 rpm, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0036] As a preferred embodiment of the present invention, the ash content of the intermediate fraction obtained by the catalytic oil slurry desolidification distillation is not higher than 10 ppm.

[0037] Compared with existing technical solutions, the present invention has at least the following beneficial effects:

[0038] (1) The present invention provides a supergravity distillation apparatus and a desolidation distillation method for desolidation of catalytic oil slurry. The apparatus and method integrate desolidation technology with vacuum distillation technology, which greatly improves the distillation efficiency and desolidation effect of catalytic oil slurry. The ash content of the intermediate fraction of catalytic oil slurry can be reduced to below 10 ppm, which can be used as a high-quality raw material for needle coke.

[0039] (2) This invention provides a supergravity distillation device and a desolidation distillation method for desolidifying catalytic oil slurry, which integrates supergravity technology and vacuum distillation technology into one device to achieve distillation cutting and effective desolidification of catalytic oil slurry; for needle coke production enterprises, it can reduce the investment and construction of filtration devices, reduce investment costs, and improve the economic benefits of enterprises. Attached Figure Description

[0040] Figure 1 This is a schematic diagram of the structure of a high-gravity distillation apparatus for catalytic desolidification of oil slurry provided in a specific embodiment of the present invention;

[0041] Figure 2 This is a schematic diagram of the feed distributor of the ultragravity distillation apparatus for catalytic desolidification of oil slurry provided in a specific embodiment of the present invention;

[0042] Figure 3 This is a schematic diagram of the quench oil feed distributor of a high gravity distillation apparatus for catalytic oil slurry desolidification provided in a specific embodiment of the present invention.

[0043] In the diagram: 1 is the distillation column; 2 is the rotating shaft; 3 is the motor; 4 is the vacuum system; 5 is the gas outlet; 6 is the rotor; 7 is the packing; 8 is the liquid collection tank; 9 is the cavity; 10 is the herringbone tray; 11 is the raw material inlet; 12 is the quench oil inlet; 13 is the coke filter; 14 is the light distillate oil outlet; 15 and 16 are the middle distillate oil outlets; 17 is the heavy distillate oil outlet.

[0044] The present invention will now be described in further detail. However, the examples described below are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention is determined by the claims. Detailed Implementation

[0045] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0046] To better illustrate the present invention and facilitate understanding of its technical solutions, typical but non-limiting embodiments of the present invention are as follows:

[0047] Example 1

[0048] This embodiment provides a high-gravity distillation apparatus for catalytic deconsolidation of oil slurry, the structure of which is as follows: Figure 1 As shown, the supergravity distillation apparatus includes a feed section, a stripping section, and a supergravity rectification section arranged sequentially.

[0049] The supergravity distillation section is equipped with a rotating shaft connected to an electric drive device. The rotating shaft has at least three rotors arranged from top to bottom. Each rotor has a first gas outlet above its connection with the rotating shaft. A sleeve is arranged along the rotating shaft as a liquid collection tank. Holes are distributed around the sleeve, and packing is arranged around the outer ring of the sleeve. A second gas outlet is arranged in the cavity formed by the first gas outlet and the tower body. The second gas outlet is connected to a condensing device, and the condensate outlet of the condensing device is connected to the liquid collection tank.

[0050] The stripping section is provided with at least two layers of herringbone trays arranged alternately.

[0051] The feeding section is provided with a catalytic oil slurry inlet and a quench oil inlet. The catalytic oil slurry inlet is connected to a catalytic oil slurry distribution device, and the quench oil inlet is connected to a quench oil distribution device. The nozzle of the quench oil distribution device is inclined downwards towards the bottom of the tower at an angle of 30 to 60°.

[0052] The supergravity distillation apparatus also includes a vacuum pumping component, and an anti-coking component is provided at the bottom of the supergravity distillation apparatus;

[0053] The bottom of the supergravity distillation apparatus is provided with an oil outlet, and the oil outlet is provided with a coke filter.

[0054] Example 2

[0055] This embodiment provides a catalytic oil slurry deconsolidation distillation method. The deconsolidation distillation method uses the high-gravity distillation apparatus for catalytic oil slurry deconsolidation provided in Example 1. The catalytic oil slurry deconsolidation distillation method includes:

[0056] The catalytic slurry is heated to 350°C and enters the feed distributor through the inlet. The vacuum system is activated, and the pressure inside the column gradually decreases to 50Pa. The motor is started, driving the rotor to rotate at a high speed of 2000rpm. The high-temperature catalytic slurry vaporizes in contact with the herringbone trays inside the column. The gas rises to the rotor and fully contacts the liquid droplets generated by the rotor for mass and heat transfer. The catalyst powder carried in the gas and liquid is thrown into the cavity under the action of gravity. As the gas rises, the amount of catalyst powder carried in the gas gradually decreases. Through the gravity separation of the three rotors and the encapsulation effect of the condensed reflux liquid on the catalyst powder during the gas-liquid contact process, most of the catalyst powder flows into the collection tank with the liquid. This effectively removes solid catalyst particles from the catalytic slurry distillate, reducing the ash content in the catalytic slurry distillate to below 10ppm. The middle distillate can be used as a high-quality feedstock for needle coke.

[0057] The heavy fraction containing a large amount of catalyst powder flows into the bottom of the distillation column. Due to the large amount of catalyst powder and the high temperature at the bottom of the column, in order to prevent coking, a low-temperature catalyst oil slurry at 120°C is injected as quench oil through the quench oil inlet. It is then fully mixed with the hot oil at the bottom of the column by the quench oil distributor. Since the nozzle of the quench oil distributor is tilted downward, it can enhance the turbulence of the liquid at the bottom of the column and reduce the temperature at the bottom of the column in time.

[0058] The coke filter installed at the bottom of the tower can block coke and prevent blockage of the heavy distillate oil pipeline at the bottom of the tower.

[0059] The properties of the catalytic slurry in Example 2 and the distillate and middle distillate obtained by desolidification and distillation are shown in Table 1.

[0060] Table 1

[0061]

[0062] The applicant declares that the detailed structural features of the present invention are illustrated through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions for the components selected in the present invention, additions of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0063] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0064] 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, the present invention will not describe the various possible combinations separately.

[0065] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.

Claims

1. A catalytic oil slurry desolidification distillation method, characterized in that, The catalytic oil slurry desolidification distillation method is carried out using a high gravity distillation device for catalytic oil slurry desolidification, which includes a feed section, a stripping section, and a high gravity rectification section arranged sequentially. The supergravity distillation section is equipped with a rotating shaft connected to an electric drive device. The rotating shaft has at least three rotors arranged from top to bottom. Each rotor has a first gas outlet above its connection with the rotating shaft. A sleeve is arranged along the rotating shaft as a liquid collection tank. Holes are distributed around the sleeve, and packing is arranged around the outer ring of the sleeve. A second gas outlet is arranged in the cavity formed by the first gas outlet and the tower body. The second gas outlet is connected to a condensing device, and the condensate outlet of the condensing device is connected to the liquid collection tank. The catalytic oil slurry desolidification and distillation method includes: The catalytic slurry enters the supergravity distillation unit via the feed section, and after being vaporized in the stripping section, it enters the supergravity rectification section. As the vaporized catalytic slurry moves upward, it sequentially contacts the droplets generated by each rotor to form a gas-liquid mixture. The catalyst powder in the gas-liquid mixture is thrown towards the cavity formed by the first gas outlet and the tower body under the action of gravity, and enters the liquid collection tank with the liquid.

2. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The stripping section is provided with at least two layers of herringbone trays arranged alternately.

3. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The feeding section is equipped with a catalytic oil slurry inlet and a quench oil inlet.

4. The catalytic oil slurry desolidification distillation method according to claim 3, characterized in that, The catalytic slurry inlet is connected to a catalytic slurry distribution device.

5. The catalytic oil slurry desolidification distillation method according to claim 3, characterized in that, The quench oil inlet is connected to a quench oil distribution device.

6. The catalytic oil slurry desolidification distillation method according to claim 5, characterized in that, The nozzle of the quench oil distribution device is inclined downwards towards the bottom of the tower at an angle of 30-60°.

7. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The supergravity distillation apparatus also includes a vacuum pumping component.

8. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The bottom of the supergravity distillation apparatus is equipped with an anti-coking component.

9. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The bottom of the supergravity distillation apparatus is provided with an oil outlet, and the oil outlet is provided with a coke filter.

10. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The feed temperature of the catalytic oil slurry is 350~370℃.

11. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The bottom temperature of the supergravity distillation apparatus is lowered by using quenching oil.

12. The catalytic oil slurry desolidification distillation method according to claim 11, characterized in that, The quenching oil is a catalytic slurry with a temperature of 100~150℃.

13. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The rotor speed is 800~3000 rpm.

14. The catalytic oil slurry desolidification distillation method according to claim 1, characterized in that, The ash content of the intermediate fraction obtained by the catalytic oil slurry desolidification distillation is not higher than 10 ppm.

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