WO2022082622A1 - Système de micro-interface d'hydrogénation - Google Patents

Système de micro-interface d'hydrogénation Download PDF

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Publication number
WO2022082622A1
WO2022082622A1 PCT/CN2020/122878 CN2020122878W WO2022082622A1 WO 2022082622 A1 WO2022082622 A1 WO 2022082622A1 CN 2020122878 W CN2020122878 W CN 2020122878W WO 2022082622 A1 WO2022082622 A1 WO 2022082622A1
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Prior art keywords
hydrogenation
micro
hydrogenation reactor
liquid
interface system
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PCT/CN2020/122878
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English (en)
Chinese (zh)
Inventor
张志炳
周政
张锋
李磊
孟为民
王宝荣
杨高东
罗华勋
杨国强
田洪舟
曹宇
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南京延长反应技术研究院有限公司
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Publication of WO2022082622A1 publication Critical patent/WO2022082622A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G75/00—Inhibiting corrosion or fouling in apparatus for treatment or conversion of hydrocarbon oils, in general

Definitions

  • the invention relates to the field of oil hydrogenation, in particular to a hydrogenation micro-interface system.
  • the existing hydrogenation reactor requires a lot of manpower in the process of maintenance and cleaning, including entering the hydrogenation reactor through the manhole for washing and on-site operation of various pipeline valves. This not only increases labor costs, but also reduces the safety of production.
  • the object of the present invention is to provide a hydrogenation micro-interface system.
  • the hydrogenation micro-interface system is provided with a liquid injector in the hydrogenation reactor.
  • the liquid injector can efficiently crush the water for cleaning the hydrogenation reactor into microns. Class droplets are smashed into the top of the hydrogenation reactor by an ejector instead of manual cleaning, so as to achieve the effect of improving mass transfer.
  • the invention provides a hydrogenation micro-interface system, comprising: a hydrogenation reactor;
  • the middle area of the bottom surface of the hydrogenation reactor protrudes upward to form a plane, and the flat parts on both sides of the protruding plane of the bottom surface of the hydrogenation reactor are respectively provided with liquid outlets, and the sidewall of the hydrogenation reactor is provided with There is a liquid inlet and a product outlet;
  • the upper part of the hydrogenation reactor is provided with a liquid injector, the bottom of the liquid injector is a plane, the top is a semicircular arc surface, and the semicircular arc surface is arranged in sequence
  • There are several injection ports the injection direction of the injection ports is toward the top of the hydrogenation reactor, and the liquid inlet is connected with the bottom of the liquid injector through a pipeline;
  • the product outlet is connected to the refining hydrogenation reactor for deep hydrogenation reaction, and the gas phase separated from the reaction product from the bottom of the refining hydrogenation reactor enters the desulfurization tower to realize the absorption of hydrogen sulfide in the gas phase.
  • the hydrogenation reactor requires a lot of manpower in the process of overhauling and cleaning, including entering the hydrogenation reactor through manholes for washing and on-site operation of various pipeline valves. This not only increases labor costs, but also reduces the safety of production.
  • the present invention provides a hydrogenation micro-interface system with a specific structure, which mainly relies on the high-efficiency crushing of the cleaning water during the spraying process of the spray port arranged on the semicircular arc surface. Mist, thereby improving the spray effect and correspondingly improving the mass transfer effect.
  • the raw materials can also be sprayed in this way during the feeding process. The raw materials are efficiently broken into mist through the spray port, thereby increasing the contact area between the raw materials, improving the reaction efficiency, and further improving the conversion rate of raw materials and yield. rate and other indicators.
  • the reason why the center of the bottom of the hydrogenation reactor is raised is to efficiently discharge the materials in the hydrogenation reactor from the liquid outlet. If the bottom is flat, there will be a small amount of material remaining, so it is best to follow the The solution of the present invention is implemented so that the center position of the bottom of the hydrogenation reactor is raised upward to form a plane.
  • the protrusions are in a semi-circular arc shape, which can further reduce the possibility of fluid accumulation.
  • the liquid outlet is set into a conical structure, which can accelerate the discharge of materials.
  • a mesh surface with a plurality of micropores evenly distributed is laid in each of the jetting openings.
  • the liquid ejector of the present invention is mainly connected with the liquid port through a pipeline, and the cleaning water is introduced into the liquid ejector and sprayed out through the ejection port on the semicircular arc surface of the liquid ejector.
  • the reason why it is designed as a semicircle The structure of the arc-shaped surface is to improve the cleaning effect and ensure that the sprayed cleaning water can clean the wall surface of the hydrogenation reactor in an all-round way. In this way, after the water sprayed out is broken and dispersed, it becomes mist to improve the mass transfer effect, which is also equivalent to the corresponding effect of the micro-interface generator.
  • the liquid inlet is connected to the central position of the bottom of the liquid ejector through a pipeline, so that the incoming liquid just enters from the middle of the liquid ejector, and the liquid can be ejected more uniformly.
  • a stirring paddle is provided at the center bulge of the inner bottom of the hydrogenation reactor to accelerate the discharge.
  • the stirring paddle is also arranged in the raised position to improve the discharge efficiency of the fermentation product, and the fermentation efficiency can also be improved by stirring.
  • two stirring paddles are arranged side by side at the protruding plane at the bottom of the hydrogenation reactor.
  • the side wall of the hydrogenation reactor is provided with a raw material inlet for entering oil products, and the raw material inlet is arranged at a lower position of the side wall of the hydrogenation reactor.
  • the oil product to be hydrogenated is introduced into the hydrogenation reactor through the raw material inlet, and the hydrogenation reaction is carried out with the introduced hydrogen to obtain the oil product after hydrodesulfurization, which ensures the quality of the product.
  • a desulfurization agent storage tank is arranged on the side of the desulfurization tower, the desulfurization agent storage tank is connected with the lower part of the side wall of the desulfurization tower through a pipeline, and the top of the desulfurization agent storage tank is connected with the desulfurization agent through a pipeline. the spray line connection.
  • the desulfurizing agent is generally lye, which is circulated into the desulfurization tower and is in reverse contact with the gas phase entering from the bottom of the desulfurization tower, sprayed and absorbed to achieve desulfurization, and the lye after desulfurization is returned to the desulfurizer storage tank. In the case of serious pollution during the recycling of the lye in the storage tank, it should be stopped for replacement.
  • the desulfurizing agent spraying pipelines are in three rows, and the desulfurizing agent spraying pipelines in each row are arranged parallel to each other.
  • the absorption effect of the desulfurizer on hydrogen sulfide in the gas phase can be improved.
  • a micro-interface generator can also be arranged in the hydrogenation reactor, and the micro-interface generator is arranged directly below the liquid injector, and the micro-interface generator is used in combination with the liquid injector to improve the synergistic effect between the two.
  • the number of the micro-interface generators is two, which are arranged in order from top to bottom.
  • the micro-interface generators are designed to be used in conjunction with each other, and the specific type is preferably a pneumatic micro-interface generator, because the pneumatic type is relatively low-cost and easy to install.
  • each of the air inlets is connected with the corresponding micro-interface generator through pipes.
  • the gas phase is sent to the desulfurization tower for desulfurization.
  • the components in the gas phase are mainly hydrogen sulfide and hydrogen. After the hydrogen sulfide is absorbed in the desulfurization tower, the hydrogen is removed from the The air inlet connected to the desulfurization tower enters into the micro-interface generator, and contacts the oil product from the raw material inlet for dispersion and crushing.
  • the micro-interface generator in the hydrogenation reactor breaks the air into micro-scale micro-bubbles and releases the micro-bubbles into the interior to increase the mass transfer area of the phase boundary between the raw materials during the reaction process, so that the two phases are fully contacted.
  • the concentration of dissolved gas in the liquid phase is increased, the efficiency is improved, and the reaction time is shortened.
  • micro-interface generator used in the present invention has been embodied in the inventor's prior patents, such as application numbers CN201610641119.6, CN201610641251.7, CN201710766435.0, CN106187660, CN105903425A, Patents of CN109437390A, CN205833127U and CN207581700U.
  • application numbers CN201610641119.6, CN201610641251.7, CN201710766435.0, CN106187660, CN105903425A, Patents of CN109437390A, CN205833127U and CN207581700U In the previous patent CN201610641119.6, the specific product structure and working principle of the micro-bubble generator (that is, the micro-interface generator) were introduced in detail.
  • the body is provided with an inlet communicating with the cavity, the opposite first and second ends of the cavity are open, wherein the cross-sectional area of the cavity is from the middle of the cavity to the first and second ends of the cavity.
  • the second end is reduced; the secondary crushing piece is arranged at at least one of the first end and the second end of the cavity, a part of the secondary crushing piece is arranged in the cavity, and both ends of the secondary crushing piece and the cavity are open
  • An annular channel is formed between the through holes of the micro-bubble generator.
  • the micro-bubble generator also includes an air inlet pipe and a liquid inlet pipe.” From the specific structure disclosed in the application document, we can know that its specific working principle is: the liquid enters the micron tangentially through the liquid inlet pipe. In the bubble generator, ultra-high-speed rotation and cutting of the gas make the gas bubbles break into micro-bubbles at the micron level, thereby increasing the mass transfer area between the liquid phase and the gas phase, and the micro-bubble generator in this patent belongs to the pneumatic micro-interface generation. device.
  • the previous patent 201610641251.7 records that the primary bubble breaker has a circulating liquid inlet, a circulating gas inlet and a gas-liquid mixture outlet, and the secondary bubble breaker communicates the feed port with the gas-liquid mixture outlet, indicating that the bubble breaker is both It needs to be mixed with gas and liquid.
  • the primary bubble breaker mainly uses circulating fluid as power, so in fact, the primary bubble breaker belongs to the hydraulic micro-interface generator, and the secondary bubble breaker is a gas-liquid breaker. The mixture is simultaneously fed into the elliptical rotating ball for rotation, so that the bubbles are broken during the rotation, so the secondary bubble breaker is actually a gas-liquid linkage type micro-interface generator.
  • micro-interface generator used in the present invention is not limited to the above-mentioned forms.
  • the specific structure of the bubble breaker described in the previous patent is only one of the forms that the micro-interface generator of the present invention can take.
  • the previous patent 201710766435.0 records that "the principle of the bubble breaker is to achieve high-speed jets to achieve gas collision", and it is also stated that it can be used in micro-interface enhanced reactors to verify the relationship between the bubble breaker and the micro-interface generator.
  • the prior patent CN106187660 also has related records for the specific structure of the bubble breaker, see specifically paragraphs [0031]-[0041] in the specification, and the accompanying drawings, which are related to the bubble breaker S-2
  • the specific working principle of the bubble breaker is described in detail.
  • the top of the bubble breaker is the liquid phase inlet, and the side is the gas phase inlet.
  • the entrainment power is provided by the liquid phase coming in from the top, so as to achieve the effect of crushing into ultra-fine bubbles, which can also be seen in the attached drawings.
  • the bubble breaker has a conical structure, and the diameter of the upper part is larger than that of the lower part, so that the liquid phase can provide better entrainment power.
  • micro-interface generator Since the micro-interface generator was just developed in the early stage of the previous patent application, it was named as micro-bubble generator (CN201610641119.6), bubble breaker (201710766435.0), etc., and later changed its name to micro-interface generator with continuous technological improvement.
  • the micro-interface generator in the present invention is equivalent to the previous micro-bubble generator, bubble breaker, etc., but the names are different.
  • the micro-interface generator of the present invention belongs to the prior art, although some micro-interface generators belong to the type of pneumatic micro-interface generators, some micro-interface generators belong to the type of hydraulic micro-interface generators, and some are of the type of hydraulic micro-interface generators. It belongs to the type of gas-liquid linkage micro-interface generator, but the difference between the types is mainly selected according to the specific working conditions.
  • the connection between the micro-interface generator and the reactor and other equipment including the connection structure, connection position, It depends on the structure of the micro-interface generator, which is not limited.
  • the hydrogenation micro-interface system of the present invention is provided with a liquid ejector in the hydrogenation reactor.
  • the liquid ejector can efficiently break the water for cleaning the hydrogenation reactor into micron-sized droplets, and collide with the ejector.
  • the upper part of the hydrogenation reactor is replaced by manual cleaning, and the raw materials actually participating in the reaction can also be efficiently broken into micron-scale droplets, so as to achieve the effect of improving the mass transfer of the reaction;
  • the hydrogenation micro-interface system of the present invention can realize the cooperation of the liquid ejector and the micro-interface generator, so that the micro-interface generator can break the air into micro-bubbles of micron scale and release the micro-bubbles into the interior,
  • the two phases are fully contacted, the concentration of the dissolved gas in the liquid phase is increased, the efficiency is improved, and the reaction time is shortened.
  • FIG. 1 is a schematic structural diagram of a hydrogenation micro-interface system provided in an embodiment of the present invention
  • FIG. 2 is a schematic structural diagram of a mesh surface of a hydrogenation micro-interface system provided by an embodiment of the present invention.
  • the terms “installed”, “connected” and “connected” should be understood in a broad sense, unless otherwise expressly specified and limited, for example, it may be a fixed connection or a detachable connection Connection, or integral connection; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium, can be internal communication between two elements.
  • installed should be understood in a broad sense, unless otherwise expressly specified and limited, for example, it may be a fixed connection or a detachable connection Connection, or integral connection; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium, can be internal communication between two elements.
  • FIG. 1 it is a hydrogenation micro-interface system according to an embodiment of the present invention, which mainly includes a hydrogenation reactor 10, a refining hydrogenation reactor 20, a desulfurization tower 30, and a desulfurization agent storage tank 40; A liquid injector 103 and a micro-interface generator 105 are provided, and the micro-interface generator 105 is arranged just below the liquid injector 103.
  • the side wall of the hydrogenation reactor 10 is provided with a liquid inlet 101 and a product outlet, and a useful For the two air inlets 106 for entering hydrogen, the liquid injector 103 is connected with the liquid inlet 101 through pipes, the bottom of the liquid injector 103 is a plane, the top surface is a semicircular arc surface, and the semicircular arc surface is A number of injection ports 1031 are arranged in sequence, and the injection direction of the injection ports 1031 is toward the top of the hydrogenation reactor 10.
  • the liquid inlet 101 is connected to the bottom of the liquid injector 103 through a pipeline, preferably by connecting with the liquid injector 103.
  • the bottom center of the liquid injector 103 is connected to the bottom center, and the liquid entering the liquid injector 103 is broken into micro-droplets with a diameter of micrometers, and ejected from the surface convex injection port 1031 to collide with the top of the hydrogenation reactor for efficient cleaning.
  • a mesh surface 1032 with a plurality of micropores evenly distributed in the spray port 1031 is laid.
  • the number of mesh surfaces 1032 is not limited. See Figure 2 for details.
  • the number of micro-interface generators 105 is two, which are arranged in order from top to bottom.
  • the two air inlets 106 are connected to the side wall of the desulfurization tower 30 for sending the purified hydrogen back to the hydrogenation reactor for further processing. It is recycled, and each air inlet 106 is connected with the corresponding micro-interface generator 105 through a pipeline.
  • the bottom of the hydrogenation reactor 10 is provided with a liquid outlet 102 for discharging the materials accumulated at the bottom of the hydrogenation reactor 10 .
  • Both sides of the bottom of the hydrogenation reactor 10 are flat, and the center position is raised upward to be a plane.
  • the liquid outlets 102 are respectively provided at the flat positions on both sides of the bottom of the hydrogenation reactor 10, and the liquid outlets 102 are used for discharging waste liquid.
  • the inner bottom center of the hydrogenation reactor 10 is provided with a stirring paddle 104 to accelerate the discharge, and the direction of the blades is upward, so as to be used for stirring at the bottom of the hydrogenation reactor 10 when flushing and draining. It can be adjusted steplessly.
  • the side wall of the hydrogenation reactor 10 is also provided with a raw material inlet 107 for entering the oil product, and the raw material inlet 107 is arranged at the lower position of the side wall of the hydrogenation reactor 10, so that the raw material inlet 107 is relatively close to the air inlet 106, The incoming oil can come into contact with hydrogen to improve the crushing and dispersing effect of hydrogen.
  • a desulfurization agent storage tank 40 is provided on the side of the desulfurization tower 30, the desulfurization agent storage tank 40 is connected with the lower part of the side wall of the desulfurization tower 30 through a pipeline, and the top of the desulfurization agent storage tank 40 is connected with the desulfurization agent spray pipeline through a pipeline, There are three rows of desulfurization agent spraying pipelines, and each row of desulfurization agent spraying pipelines is arranged in parallel with each other.
  • This embodiment also includes a PLC (or DCS, PLC and DCS) control system: connected to the sensor of the hydrogenation reactor 10, for intelligently controlling process operations and parameters, realizing remote control of production, in line with the intelligentization of production .
  • PLC or DCS, PLC and DCS
  • the cleaning water above the hydrogenation reactor 10 is transported to the inside of the liquid ejector 103 through the liquid inlet 101 and sprayed out through the jetting port 1031 on the arc surface, and is efficiently broken into microns through the mesh surface 1032
  • the liquid droplets of the order (1 ⁇ m ⁇ d ⁇ 1 mm) are ejected from the protruding ejection port 1031 on the surface of the liquid ejector 103 , collide with the top of the hydrogenation reactor 10 and clean the top.
  • the cleaned droplets form a liquid level at the bottom of the tank.
  • the installation direction of the blades of the stirring paddle 104 is downward, the liquid above the blades will be pumped to the two sides below, and vortices will be formed on both sides of the stirring paddle 104 to wash and clean both sides of the lower part of the hydrogenation reactor 10 .
  • the water channel below is opened, and the input water flow cleans the side wall of the hydrogenation reactor under the action of the stirring paddle 104, closes the water delivery valve after flushing for 30 minutes, reduces the rotational speed to 100rpm/min, and passes through the lower end of the hydrogenation reactor 10.
  • the liquid outlets 102 on both sides discharge water, close the liquid outlets 102, and reduce the rotational speed to 50 rpm/min.
  • the operation and process parameters in the working process of the above-mentioned hydrogenation micro-interface system are completely controlled by the control system of PLC (or DCS, PLC and DCS), and the control system is connected with each sensor on the hydrogenation reactor 10 to realize automatic intelligent control, Save labor costs.
  • the pressure of the above hydrogenation reaction is 2-8MPa, and the temperature of the hydrogenation reaction is 250-320°C. Most preferably, the pressure of the hydrogenation reaction is 3.5 MPa, and the temperature of the hydrogenation reaction is 300°C.
  • the pressure of the refining hydrogenation reaction is 2-8MPa, and the temperature of the refining hydrogenation reaction is 250-320°C. Most preferably, the pressure of the refining hydrogenation reaction is 3.5MPa, and the temperature of the refining hydrogenation reaction is 300°C.
  • the catalyst used in both the hydrogenation reaction and the refining hydrogenation reaction is a Mo-Ni type catalyst, and the volume ratio of the catalyst dosage in the hydrogenation reactor 10 and the refining hydrogenation reactor 20 can be (1:12)-(1:15) , preferably 1:13.
  • the solution of the present invention realizes not only the dispersion and crushing of the liquid phase, but also the dispersion and crushing of the gas phase through the cooperation of the liquid ejector and the micro-interface generator. particles, so as to improve the mass transfer effect of the system.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

La présente divulgation concerne un système de micro-interface d'hydrogénation, comprenant un réacteur d'hydrogénation. Une région centrale au niveau de la surface inférieure du réacteur d'hydrogénation fait saillie vers le haut pour former un plan. Des sorties de liquide sont respectivement agencées au niveau de parties plates sur deux côtés du plan qui fait saillie à partir de la surface inférieure du réacteur d'hydrogénation. Une entrée de liquide et une sortie de produit sont disposées sur une paroi latérale du réacteur d'hydrogénation. Un jet de liquide est disposé au niveau d'une partie supérieure dans le réacteur d'hydrogénation. La partie inférieure du jet de liquide est un plan, et la partie supérieure du jet de liquide a une surface d'arc semi-circulaire. Plusieurs orifices d'éjection sont disposés en séquence sur la surface d'arc semi-circulaire et ont des directions d'éjection faisant face à la partie supérieure du réacteur d'hydrogénation. L'entrée de liquide est reliée à la partie inférieure du jet de liquide au moyen d'une canalisation. La sortie de produit est reliée à un réacteur d'hydrogénation affiné pour effectuer une réaction d'hydrogénation profonde. Une phase gazeuse séparée d'un produit de réaction de la partie inférieure du réacteur d'hydrogénation raffiné entre dans une colonne de désulfuration de sorte que le sulfure d'hydrogène dans la phase gazeuse est absorbé. Le système de micro-interface d'hydrogénation de la présente divulgation permet d'économiser le coût des opérations de nettoyage et sur site.
PCT/CN2020/122878 2020-10-21 2020-10-22 Système de micro-interface d'hydrogénation WO2022082622A1 (fr)

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CN113058517B (zh) * 2021-03-23 2023-05-05 南京延长反应技术研究院有限公司 一种丁辛醇的微界面制备装置及方法
CN113045387A (zh) * 2021-03-23 2021-06-29 南京延长反应技术研究院有限公司 一种丙烯羰基化制丁辛醇的反应系统及方法

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