WO2020186637A1 - Système d'hydrogénation à lit fluidisé de renforcement à micro-interface - Google Patents

Système d'hydrogénation à lit fluidisé de renforcement à micro-interface Download PDF

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Publication number
WO2020186637A1
WO2020186637A1 PCT/CN2019/090280 CN2019090280W WO2020186637A1 WO 2020186637 A1 WO2020186637 A1 WO 2020186637A1 CN 2019090280 W CN2019090280 W CN 2019090280W WO 2020186637 A1 WO2020186637 A1 WO 2020186637A1
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micro
gas
reaction
liquid
hydrogen
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PCT/CN2019/090280
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English (en)
Chinese (zh)
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张志炳
周政
孟为民
王宝荣
杨高东
罗华勋
张锋
李磊
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 WO2020186637A1 publication Critical patent/WO2020186637A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
    • B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/02—Feed or outlet devices therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/001—Controlling catalytic processes
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
    • C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
    • C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
    • C10G45/08—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/202—Heteroatoms content, i.e. S, N, O, P
    • 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/70—Catalyst aspects

Definitions

  • the invention relates to the technical field of fluidized bed hydrogenation, in particular to a micro-interface enhanced fluidized bed hydrogenation reaction system.
  • the fluidized bed reactor is a kind of reactor that uses gas or liquid to pass through the granular solid layer to make the solid particles in a suspended state, and carry out the gas, liquid, and solid three-phase mutual reaction. Since the catalyst can realize online replacement, continuous regeneration and recycling operation, it is very suitable for processing heavy and inferior feedstock oils with high metal content and high asphaltene content. In addition, the fluidized bed reactor has the advantages of large space velocity, small pressure drop in the reactor, uniform temperature distribution, good mass and heat transfer, high catalyst utilization, long operation period, and flexible device operation. It overcomes the shortcomings of a rapid rise in bed pressure drop due to carbon deposits and metal deposition on the catalyst in the fluidized bed hydrogenation process.
  • the current industrial application is mainly the typical fluidized bed reactor described in US Re 25,770, but this reactor process has the following shortcomings in practical applications: the catalyst storage in the reactor is small, and the space utilization rate of the reactor is low. The reaction efficiency is reduced; the maintenance cost of the circulating oil pump is high, and once the circulating oil pump works abnormally and damaged, the catalyst will sink and accumulate, which will force the device to shut down; the liquid product in the reactor stays under non-catalytic hydrogenation conditions If the time is too long, it is easy to carry out the second thermal cracking reaction and coking at high temperature, which will reduce the product quality.
  • the operation of this component requires that the gas, solid, and liquid three-phase linear velocity in the separation section be equal or lower than the linear velocity of the reactor, so the reactor is equipped with a three-phase separator cylinder
  • the diameter of the body is larger than the diameter of the reactor, which increases the volume of the reactor. Because the reactor is a high-temperature and high-pressure equipment, the diameter-expanding structure brings difficulties to the manufacture of the equipment.
  • Cipheral Patent Publication Number: CN104946307A discloses a fluidized bed hydrogenation device, including a heating furnace, a first fluidized bed residue hydrogenation reactor, a second fluidized bed residue hydrogenation reactor, and thermal high separation gas/mixed hydrogen exchange Heater, cold high-pressure separator, circulating hydrogen compressor, the outlet of the heating furnace is connected to the bottom inlet of the first boiling-bed residue hydrogenation reactor, and the upper outlet of the first boiling-bed residue hydrogenation reactor is connected to the second boiling
  • the bottom inlet of the bed residue hydrogenation reactor is connected, and the top outlets of the first fluidized bed residue hydrogenation reactor and the second fluidized bed residue hydrogenation reactor are both connected with the hot high separation gas/mixed hydrogen heat exchanger,
  • the hot high separation gas/mixed hydrogen heat exchanger is connected to the circulating hydrogen compressor, the hot high separation gas/mixed hydrogen heat exchanger is connected to the cold high-pressure separator through the high-pressure air cooler, and the cold high-pressure separator is connected to the circulating hydrogen pur
  • the device has the following problems:
  • the hydrogen pressure used by the device during operation is too large, which has potential safety hazards during operation, and requires a large amount of resources to be consumed, and the process operation cost is high.
  • the device in order to ensure the activity of the catalyst, the device requires a higher reaction temperature. While increasing the reaction temperature in the fluidized bed, the energy consumption of the process is further increased.
  • the device only mixes hydrogen with the reaction medium, so that the hydrogen molecules cannot be sufficiently mixed with the reaction medium, resulting in a decrease in reaction efficiency.
  • the olefins in the reaction medium in the device are prone to saturation under hydrodesulfurization conditions, which not only consumes a large amount of hydrogen, but also reduces the octane number of the reaction medium and the operating conditions are harsh.
  • the present invention provides a micro-interface enhanced fluidized bed hydrogenation reaction system to overcome the problem of excessively high process energy consumption due to the inability of hydrogen to fully contact the reaction medium in the prior art.
  • the present invention provides a micro-interface enhanced fluidized bed hydrogenation reaction system, which includes:
  • Liquid phase feeding unit to store and transport the reaction medium
  • Gas phase feeding unit for storing and transporting hydrogen
  • At least one Micro Interfacial Generator which is respectively connected with the liquid phase feeding unit and the gas phase feeding unit, and converts the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubble and transmits it Give hydrogen bubbles to break the hydrogen to form micro-bubbles with a diameter greater than or equal to 1 ⁇ m and less than 1 mm to increase the mass transfer area between the reaction medium and hydrogen, and mix the reaction medium with the micro-bubbles to form a gas-liquid emulsion after crushing.
  • MIG Micro Interfacial Generator
  • a fluidized bed reactor which is connected to the micro-interface generator and is used for loading the gas-liquid emulsion and providing a reaction space for the reaction medium and microbubbles in the gas-liquid emulsion;
  • the separation tank is used to separate the gas-liquid mixture of the reaction medium and the mixed gas after the reaction is completed in the fluidized bed reactor.
  • the micro-interface generators are arranged in parallel and the arrangement of the micro-interface generators is one or more of series, parallel and mixed connection , Used to output the mixed gas-liquid emulsion to the fluidized bed reactor for reaction.
  • micro-interface generator is one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
  • liquid phase feeding unit includes:
  • Liquid raw material tank to store the reaction medium
  • a feed pump connected to the liquid raw material tank to provide power for the transportation of the reaction medium
  • the liquid feed preheater which is connected to the feed pump, is used to preheat the reaction medium delivered by the feed pump so that the reaction medium reaches a specified temperature, and the liquid feed preheater is provided at the outlet There are shunt pipes to transport the reaction medium to the corresponding micro-interface generators respectively;
  • the feeding pump starts to operate, and the reaction medium is drawn out from the liquid raw material tank and delivered to the liquid feed preheater, and the liquid feed is preheated
  • the reactor heats the reaction medium to a specified temperature and then delivers the reaction medium to the micro-interface generator.
  • gas phase feed unit includes:
  • a compressor which is connected to the gas raw material buffer tank to provide power for the transmission of hydrogen
  • a gas feed preheater which is connected to the compressor, and is used to preheat the hydrogen delivered by the compressor to make the hydrogen reach a specified temperature, and a split pipeline is provided at the outlet of the gas feed preheater, Used to deliver hydrogen to the corresponding micro-interface generators;
  • the compressor starts to operate, and the hydrogen is pumped out of the gas raw material buffer tank and delivered to the gas feed preheater for preheating. After the preheating is completed, the gas The feed preheater delivers hydrogen to the micro-interface generator so that the micro-interface generator breaks the hydrogen to a specified size.
  • the fluidized bed reactor includes:
  • the reaction tank which is a tank body, is used to provide a reaction space for the gas-liquid emulsion, and the upper part of the reaction tank is provided with a discharge port for outputting the reacted medium and mixed gas after the reaction;
  • the distribution plate is arranged in the reaction tank, and a catalyst is arranged on its surface to promote the reaction of various substances in the gas-liquid emulsion;
  • a catalyst feed pipe which is arranged on the top of the reaction tank to transport the catalyst to the distribution plate;
  • the catalyst discharging pipe is arranged at the bottom of the distribution plate and connected to it, and is used to discharge the deactivated catalyst out of the reaction tank.
  • the top of the separation tank is provided with a gas-phase outlet for conveying mixed gas
  • the bottom of the separation tank is provided with a liquid-phase outlet for conveying the post-reaction medium.
  • the beneficial effect of the present invention is that compared with the traditional fluidized bed reactor, the present invention breaks the gas to form micro-sized micro-bubbles and mixes the micro-bubbles with the reaction medium to form a gas-liquid emulsion.
  • the pressure in the reaction process can be reduced by 10-80%; at the same time, the present invention
  • the gas-liquid ratio can be greatly reduced, which not only reduces the material consumption of the gas, but also reduces the energy consumption of the subsequent gas cycle compression; and the method of the present invention has low process severity and production safety High, low cost per ton product, strong market competitiveness.
  • the system of the present invention uses different catalysts, the operating temperature will be adjusted appropriately according to the active temperature of the catalyst. Therefore, the system of the present invention also has the ability to significantly or exponentially reduce the operating temperature under different catalyst systems. Pressure and increase the space velocity (handling capacity) advantage.
  • the micron-sized bubbles collide with the movement of the catalyst particles, they are not prone to coalescence and can basically maintain their original shape. Therefore, the contact area between the gas phase and the liquid phase in the fluidized bed reactor is increased geometrically, and the emulsification and mixing are more sufficient and stable, so as to achieve the effect of enhancing mass transfer and macro-reaction.
  • liquid-phase feeding unit and the gas-phase feeding unit are respectively provided with a feed pump and a compressor, so that when the system is running, the feed pump and the compressor can respectively transport the reaction medium and hydrogen. Power is provided so that the reaction medium and hydrogen can be delivered to the designated device at a designated rate, which improves the operating efficiency of the system.
  • the liquid-phase feed unit and the gas-phase feed unit are respectively provided with a liquid feed preheater and a gas feed preheater.
  • the liquid feed preheater and The gas feed preheater can separately preheat the reaction medium and hydrogen.
  • the fluidized bed reactor does not need to heat the reaction medium and hydrogen with high power during operation, which saves the resource consumption of the fluidized bed. , Which reduces the energy consumption of the system.
  • the system is provided with at least one micro-interface generator, so that the system can fully mix the reaction medium and hydrogen in different proportions by using a plurality of micro-interface generators, and can significantly react with the catalyst. Improve the reaction efficiency of each substance in the gas-liquid emulsion.
  • the fluidized bed reactor is provided with a catalyst inlet and a catalyst outlet.
  • the reaction rate inside the fluidized bed reactor can be maintained at a specified threshold, thereby Further improve the operating efficiency of the system.
  • the separation tank can separate the reacted mixture into gas and liquid by using gravity, without using redundant separation devices for the separation tank, which further reduces the energy consumption of the system.
  • Figure 1 is a schematic diagram of the structure of the bottom micro-interface enhanced fluidized bed hydrogenation reaction system of the present invention
  • Figure 2 is a schematic structural diagram of the side-opposed micro-interface enhanced fluidized bed hydrogenation reaction system of the present invention.
  • connection should be understood in a broad sense.
  • it can be a fluidized bed connection or It can be a detachable connection or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication between two components.
  • connection should be understood in a broad sense.
  • it can be a fluidized bed connection or It can be a detachable connection or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication between two components.
  • FIG. 1 is a schematic structural diagram of a downward-mounted micro-interface enhanced boiling bed hydrogenation reaction system according to an embodiment of the present invention, including a liquid feeding unit 1, a gas feeding unit 2, a micro-interface generator 3 (Micro Interfacial Generator, MIG for short), fluidized bed reactor 4 and separation tank 5; wherein, the micro-interface generator 3 is connected to the liquid feed unit 1 and the gas feed unit 2 respectively to receive the liquid feed The reaction medium delivered by the feeding unit 1 and the hydrogen delivered by the gas feeding unit 2; the fluidized bed reactor 4 is connected to the micro-interface generator 3, and the output end of the micro-interface generator 3 is set inside the fluidized bed reactor 4 , Used to output the gas-liquid emulsion in the micro-interface generator 3 to the fluidized bed reactor; the separation tank 5 is connected to the fluidized bed reactor 4 to receive the mixture output from the fluidized bed reactor 4 and The mixture undergoes gas-liquid separation.
  • MIG Micro Interfacial Generator
  • the liquid feeding unit 1 When the system is running, the liquid feeding unit 1 is activated and the reaction medium stored in it is transported to the micro-interface generator 3, and at the same time the gas feeding unit 2 is activated, and the stored internally
  • the hydrogen is delivered to the micro-interface generator 3, and the micro-interface generator 3 breaks the hydrogen to a micrometer scale to form micro-bubbles with a diameter greater than or equal to 1 ⁇ m and less than 1 mm.
  • the micro-interface After the crushing is completed, the micro-interface occurs
  • the device 3 mixes the microbubbles with the reaction medium to form a gas-liquid emulsion.
  • the micro-interface generator 3 outputs the gas-liquid emulsion to the fluidized bed reactor 4 after the gas-liquid emulsion is mixed.
  • the temperature and air pressure enable the gas-liquid emulsion to react efficiently in the ebullating-bed reactor.
  • the ebullating-bed reactor 4 outputs the resulting mixture to the separation tank 5, and the separation tank 5 combines the reacted medium in the mixture with hydrogen and
  • the mixed gas of hydrogen sulfide is separated and processed separately.
  • the system of the present invention can be used to hydrogenate gasoline, diesel, wax oil, lubricating oil or other types of oil, as long as the system is capable of hydrogenating oil.
  • the oil can react efficiently and reach the specified standard after the reaction.
  • system of the present invention can also be used in other multi-phase reactions, such as through micro-interface, micro-nano interface, ultra-micro interface, micro-bubble bioreactor or micro-bubble bioreactor and other equipment, using micro-mixing, micro-fluidization , Ultra-micro fluidization, micro-bubble fermentation, micro-bubble, micro-bubble mass transfer, micro-bubble transfer, micro-bubble reaction, micro-bubble absorption, micro-bubble oxygenation, micro-bubble contact and other processes or methods to make the material form more Phase micro-mixed flow, multi-phase micro-nano flow, multi-phase emulsified flow, multi-phase micro-structured flow, gas-liquid-solid micro-mixed flow, gas-liquid-solid micro-nano flow, gas-liquid-solid emulsified flow, gas-liquid-solid microstructure flow, microbubbles, Micro-bubble flow, micro-bubble, micro-bubble flow, micro-liquid flow, gas-liquid micro-nan
  • the liquid feed unit 1 includes: a liquid raw material tank 11, a feed pump 12, and a liquid feed preheater 13; wherein, the feed pump 12 and the The liquid raw material tank 11 is connected to extract the reaction medium in the liquid raw material tank 11; the liquid feed preheater 13 is arranged at the output end of the feed pump 12 and the liquid feed preheater 13 is connected to the The micro-interface generator 3 is connected to preheat the reaction medium output by the feed pump 12 and deliver the reaction medium to the micro-interface generator 3 after preheating.
  • the feed pump 12 When the liquid feed unit 1 is operating, the feed pump 12 will extract the reaction medium stored in the liquid raw material tank 11 and deliver it to the liquid feed preheater 13, and the liquid feed is preheated After the reactor 13 preheats the reaction medium to a specified temperature, the reaction medium is transported to the micro-interface generator 3.
  • the liquid raw material tank 11 is a tank body for storing the reaction medium, and the liquid raw material tank 11 is connected with the feed pump 12 to transport the reaction medium through the feed pump 12 when the system is running. To the specified location. It is understandable that the liquid raw material tank 11 may be a metal oil tank or a non-metal oil tank, as long as the liquid raw material tank 11 can be loaded with a specified amount of reaction medium.
  • the feed pump 12 is a centrifugal pump, which is arranged at the outlet of the liquid raw material tank 11 to provide power for the transportation of the reaction medium.
  • the feed pump 12 starts to run to pump out the reaction medium in the liquid raw material tank 1 and deliver it to the liquid feed preheating unit 13. It can be understood that the model and power of the feed pump 12 are not specifically limited in this embodiment, as long as the feed pump 12 can deliver the reaction medium at a specified flow rate.
  • the liquid feed preheater 13 is a preheater for preheating the reaction medium, and the outlet of the liquid feed preheater 13 is provided with a shunt pipe to heat the preheated reaction
  • the medium is respectively delivered to the inside of each of the micro-interface generators.
  • the feed pump 12 transports the reaction medium
  • the reaction medium will flow through the liquid feed preheater 13, and the liquid feed preheater 13 will preheat the reaction medium and divide the flow after the reaction medium reaches a specified temperature.
  • the reaction medium is respectively transported to the inside of each micro-interface generator.
  • the type of preheater and heating method of the liquid feed preheater 13 are not specifically limited in this embodiment, as long as the liquid feed preheater 13 can preheat the reaction medium to a specified temperature. OK.
  • the gas feeding unit 2 includes: a gas raw material buffer tank 21, a compressor 22, and a gas feed preheater 23; wherein, the compressor 22 and the gas
  • the raw material buffer tank 21 is connected to extract the hydrogen in the gas raw material buffer tank 21;
  • the gas feed preheater 23 is arranged at the output end of the compressor 22 and the gas feed preheater 23 is connected to the micro
  • the interface generator 3 is connected to preheat the hydrogen output from the compressor 22 and deliver the hydrogen to the micro interface generator 3 after the preheating.
  • the compressor 22 When the gas feed unit 2 is running, the compressor 22 will extract the hydrogen stored in the gas raw material buffer tank 21 and deliver it to the gas feed preheater 23, which is a gas feed preheater 23 After preheating the hydrogen to a specified temperature, the hydrogen is delivered to the micro-interface generator 3.
  • the gas raw material buffer tank 21 is a tank body for storing hydrogen gas, and the gas raw material buffer tank 21 is connected to the compressor 22 to deliver hydrogen gas to the designated destination through the compressor 22 when the system is running. position. It is understandable that the type of the gas raw material buffer tank 21 is not specifically limited in this embodiment, as long as the gas raw material buffer tank 21 can be loaded with a specified amount of hydrogen.
  • the compressor 22 is arranged at the outlet of the gas raw material buffer tank 21 to provide power for the transmission of hydrogen.
  • the compressor 22 starts to operate to extract the hydrogen in the gas raw material tank 2 and deliver it to the gas feed preheating unit 23.
  • the power of the compressor 22 is not specifically limited in this embodiment, as long as the compressor 22 can deliver hydrogen at a specified flow rate.
  • the gas feed preheater 23 is a preheater for preheating hydrogen, and the outlet of the gas feed preheater 23 is provided with a branch pipe to separate the preheated hydrogen. Transported to the inside of each of the micro-interface generators.
  • the compressor 22 delivers hydrogen
  • the hydrogen will flow through the gas feed preheater 23, and the gas feed preheater 23 will preheat the hydrogen and split the flow when the hydrogen reaches a specified temperature, and deliver the hydrogen to Inside each micro-interface generator.
  • the type of preheater and heating method of the gas feed preheater 23 are not specifically limited in this embodiment, as long as the gas feed preheater 23 can preheat hydrogen to a specified temperature. can.
  • the micro-interface generator 3 of the present invention includes a first micro-interface generator 31 and a second micro-interface generator 32, the first micro-interface generator 31 and the second micro-interface generator 32 is vertically arranged at the bottom of the fluidized bed reactor 4, and the first micro-interface generator 31 and the second micro-interface generator 32 are parallel to each other, and the output ports of each micro-interface generator are arranged inside the fluidized bed reactor 4, In order to output the gas-liquid emulsion to the fluidized bed reactor 4.
  • the first micro-interface generator 31 and the second micro-interface generator 32 will receive a specified amount of reaction medium and hydrogen, respectively.
  • the first micro-interface generator 31 and The second micro-interface generator 32 breaks the received hydrogen and breaks the hydrogen to a micron size to form microbubbles.
  • the microbubbles are mixed with the reaction medium to form a gas-liquid emulsion, and the gas-liquid emulsion is output after the mixing is completed To the boiling bed reactor 4.
  • the connection between the micro-interface generator 3 and the fixed-bed reactor 4 can be pipe connection, the output end of the micro-interface generator 3 is set inside the fixed-bed reactor 4 or other types of connections Mode, as long as it is satisfied that the micro-interface generator 3 can output the gas-liquid emulsion to the inside 4 of the fixed bed reactor.
  • the first micro-interface generator 31 is a gas-liquid linkage type micro-interface generator, which is arranged at the bottom of the fluidized bed reactor 4 and is respectively connected with the liquid feed preheater 13 and the gas feed preheater.
  • the heat exchanger 23 is connected to break the hydrogen gas and output the gas-liquid emulsion formed by mixing the microbubbles and the reaction medium to the inside of the boiling bed reactor 4.
  • the first micro-interface generator 31 will respectively receive a specified amount of reaction medium and hydrogen, and use the pressure energy of the gas and the kinetic energy of the liquid to break the hydrogen bubbles to the micrometer scale.
  • the microbubbles and the reaction medium are mixed vigorously to form a gas-liquid emulsion, and the gas-liquid emulsion is output to the fluidized bed reactor 4 after the mixing is completed.
  • the second micro-interface generator 32 is a pneumatic micro-interface generator, which is arranged at the bottom of the fluidized bed reactor 4 and is respectively preheated with the liquid feed preheater 13 and the gas feed
  • the device 23 is connected to break the hydrogen gas and output the gas-liquid emulsion formed by mixing the microbubbles and the reaction medium to the inside of the boiling bed reactor 4.
  • the first micro-interface generator 31 will respectively receive a specified amount of reaction medium and hydrogen, and use the pressure of the gas to break the hydrogen bubbles to the micrometer scale.
  • the reaction medium is mixed vigorously to form a gas-liquid emulsion, and the gas-liquid emulsion is output to the boiling bed reactor 4 after the mixing is completed.
  • the fluidized bed reactor 4 includes a reaction tank 41, a distribution plate 42, a catalyst feed port 43 and a catalyst discharge port 44; wherein the distribution plate 42 is arranged in the reaction tank
  • the inside of 41 is used for loading catalyst;
  • the catalyst feed port 43 is set on the top of the reaction tank 41 to transport fresh catalyst;
  • the catalyst discharge port 44 is opened at the bottom of the reaction tank 41 and is connected to the
  • the distribution plate 42 is connected to output the deactivated catalyst in the reaction tank 41.
  • the micro-interface generator 3 When the fluidized bed reactor 4 is running, the micro-interface generator 3 will output the gas-liquid emulsion to the bottom of the reaction tank 41, and the gas-liquid emulsion will gradually flow upwards after entering the bottom of the reaction tank 41, and the gas-liquid emulsification
  • the substance flows through the distribution plate 42 during the flow process, drives the catalyst on the surface 42 of the distribution plate and starts to react, so that the sulfur element contained in the reaction medium in the gas-liquid emulsion reacts with the microbubbles to generate hydrogen sulfide; the catalyst is in the gas-liquid emulsion During the irregular flow, the abrasion occurs, and after a certain period of time, the deactivated catalyst will sink to the distribution plate 42.
  • the catalyst discharge port 44 will output the catalyst to the reaction tank 41, and the catalyst feed port 43
  • the fresh catalyst is delivered to the inside of the reaction tank 41 to ensure the reaction rate of the reaction medium and the microbubbles in the gas-liquid emulsion.
  • the catalyst can be one or a mixture of molybdenum-based catalysts, cobalt-based catalysts, tungsten-based catalysts, nickel-based catalysts, and iron-based catalysts, as long as the catalyst can improve the gas-liquid emulsion The reaction efficiency of each substance is sufficient.
  • the present invention is applicable to the above mentioned catalyst systems as well as other hydrogenation catalyst systems not mentioned.
  • the operating temperature will be based on the active temperature of the catalyst used.
  • the parallel system has the ability to greatly or double the operating pressure and increase the space velocity (processing capacity) under different catalyst systems.
  • the reaction tank 41 is a cylindrical metal tank with an inlet at the bottom for receiving the gas-liquid emulsion output by the micro-interface generator 3, and an outlet at the top.
  • the discharging port is connected with the separation tank 5 for outputting the reaction-completed mixture to the separation tank 5 for gas-liquid separation.
  • the feed port of the reaction tank 41 will receive the gas-liquid emulsion output by the micro-interface generator 3 and provide a reaction space for the gas-liquid emulsion.
  • a mixture of the post-reaction medium and the mixed gas is formed, and the reaction tank 41 will output the mixture to the separation tank 5 through the discharge port.
  • reaction tank 41 the size and material of the reaction tank 41 are not specifically limited in this embodiment, as long as the reaction tank 41 can be loaded with a specified amount of gas-liquid emulsion and has a specified strength to withstand the preset reaction temperature and Just react to pressure.
  • the distribution plate 42 is a layer of sieve plate, which is arranged at the bottom of the reaction tank 41 to contain the catalyst.
  • the gas-liquid emulsion in the reaction tank 41 will flow upwards from the bottom of the reaction tank 41 and pass through the distribution plate 42 during the flow.
  • the catalyst separates from the distribution plate, moves irregularly inside the gas-liquid emulsion and promotes the reaction between the reaction medium and the microbubbles in the gas-liquid emulsion.
  • the distribution plate 42 can be a grid, a screen, a ceramic ball or other types of structures, as long as the distribution plate 42 can reach its designated working state.
  • the catalyst feed pipe 43 is a cylindrical metal pipe, which is arranged on the top of the reaction tank 41 to transport fresh catalyst into the reaction tank 41.
  • the catalyst in the gas-liquid emulsion will continue to move irregularly, causing friction, which will cause the catalyst to deactivate and reduce the reaction efficiency inside the reaction tank 41.
  • the catalyst The feed pipe will transport the fresh catalyst to the inside of the reaction tank 41 to ensure the reaction efficiency of the reaction medium and microbubbles.
  • the catalyst discharge pipe 44 is a cylindrical metal pipe, which is arranged at the bottom of the reaction tank 41, and its upper end is connected with the distribution plate 42 for deactivating the sedimentation on the distribution plate 42 Catalyst output.
  • the catalysts in the reaction tank 41 move irregularly, they will rub against each other and be damaged and lose their activity.
  • the inactive catalyst will settle on the distribution plate 42.
  • the catalyst discharge pipe 44 will affect the deactivated catalyst. Accumulate and output.
  • the separation tank 5 is a metal tank body, which is connected to the discharge port of the reaction tank 41, and is used to perform gas-liquid gasification on the mixture output from the reaction tank 41. Separate.
  • the separation tank 5 is provided with a gas phase outlet at the top for outputting hydrogen and hydrogen sulfide gas, and a liquid phase outlet at the bottom for outputting the reaction medium.
  • the separation tank 5 will use gravity to separate the mixed gas in the mixture from the reaction medium, and will contain hydrogen and sulfur.
  • the mixed gas of hydrogen gas is output through the gas phase outlet, and the reacted medium is output through the liquid phase outlet.
  • the size and material of the separation tank 5 are not specifically limited in this embodiment, as long as the separation tank 5 has a specified strength and can be loaded with a mixture of a specified volume.
  • FIG. 2 is a schematic structural diagram of a side opposed micro-interface enhanced fluidized bed hydrogenation reaction system according to an embodiment of the present invention.
  • the components used in the system are the same as those in the first embodiment of the system.
  • the micro-interface generator 3 is also provided with a third micro-interface generator 33, and the third micro-interface generator 33 is set in the gas feed forecast.
  • the third micro-interface generator 33 is connected in parallel with the second micro-interface generator 32 to break a specified amount of hydrogen; the third micro-interface generator 33 is also connected to the first
  • a micro-interface generator 31 is connected in series to break the hydrogen gas in multiple stages, thereby further reducing the diameter of the microbubbles.
  • the first micro-interface generator 31 and the second micro-interface generator 32 are respectively arranged on the side wall of the bottom of the reaction tank 4, and the first micro-interface generator 31 and the second micro-interface generator 32 are paired It is arranged to make the first micro-interface generator 31 and the second micro-interface generator 32 impact each other when outputting the gas-liquid emulsion, so that the gas-liquid emulsion is mixed more uniformly.
  • the third micro-interface generator 33 and the second micro-interface generator 32 will respectively receive The specified amount of reaction medium and hydrogen is crushed to the micron size to form microbubbles and the reaction medium is mixed with the microbubbles to form a gas-liquid emulsion. After crushing, the third micro-interface generator 33 will transport the gas-liquid emulsion to The first micro-interface generator 31 is further broken.
  • the first micro-interface generator 31 and the second micro-interface generator 32 will output the internal gas-liquid emulsion to the bottom of the reaction tank 41 and Moving from bottom to top, because the two micro-interface generators are arranged oppositely, when the second micro-interface generator 32 and the third micro-interface generator 33 output gas-liquid emulsion, two streams of gas-liquid emulsion fluid will be The bottom of the reaction tank 41 is hedged to achieve secondary mixing of the gas-liquid emulsion, so as to further increase the mass transfer area of the reaction medium and the microbubbles between the gas-liquid emulsion.
  • a reaction method of a bottom-mounted micro-interface enhanced fluidized bed hydrogenation reaction system comprising the following steps:
  • Step 1 Before operating the system, add a specified amount of reaction medium to the liquid raw material tank 11, and add a specified amount of hydrogen to the gas raw material buffer tank 21;
  • Step 2 Start the system after the addition is completed, extract the reaction medium from the liquid raw material tank 11 through the feed pump 12, and extract hydrogen from the gas raw material buffer tank 21 through the compressor 22;
  • Step 3 The reaction medium flows through the liquid feed preheater 13, the liquid feed preheater 13 heats the reaction medium to a specified temperature, the hydrogen flows through the gas feed preheater 23, and the gas feed preheater 23 heats the hydrogen Heat to the specified temperature;
  • Step 4 The reaction medium is split after preheating.
  • the split reaction medium will be delivered to the corresponding micro-interface generator.
  • the hydrogen will be split after preheating, and the split hydrogen will be delivered to the corresponding micro-interface.
  • Step 5 Each of the micro-interface generators controls the ratio between the receiving reaction medium and hydrogen, and breaks the hydrogen to micrometer scale to form micro-bubbles. After the break is completed, each of the micro-interface generators Microbubbles and reaction medium are mixed to form gas-liquid emulsion;
  • Step 6 Each of the micro-interface generators outputs the gas-liquid emulsion to the fluidized bed reactor 4 after the mixing is completed, controls the pressure and temperature in the fluidized-bed reactor, and makes the gas-liquid emulsion flow in a designated direction;
  • Step 7 The gas-liquid emulsion flows through the distribution plate 42 to mix the catalyst provided on the distribution plate 42 with the gas-liquid emulsion, so that the catalyst promotes the reaction between the sulfur element in the reaction medium in the gas-liquid emulsion and the microbubbles. Generate reaction medium and hydrogen sulfide gas to desulfurize and upgrade the reaction medium, and hydrogen sulfide gas will form a mixed gas with hydrogen;
  • Step 8 After the reaction is completed, the fluidized bed reactor 4 transports the mixture formed by the reacted medium and the mixed gas to the separation tank 5. The mixture settles in the separation tank 5. After the reaction, the medium settles in the lower layer of the separation tank 5 and is The liquid phase outlet is output from the system for subsequent processing, and the mixed gas stays in the upper layer of the separation tank 5 after the medium settles after the reaction and is output from the system through the gas phase outlet for subsequent processing.
  • each of the micro-interface generators in the step 5 generates micro-bubbles with an average diameter greater than or equal to 1 ⁇ m and less than 1 mm after the hydrogen gas is broken.
  • the standard volume ratio of hydrogen to FCC gasoline in the first micro-interface generator is 0.25:1; the standard volume ratio of hydrogen to FCC gasoline in the second micro-interface generator is 800:1.
  • the air pressure inside the fluidized bed reactor 4 is controlled at 3 MPa, the reaction temperature is controlled at 220° C., and the space velocity is controlled at 0.5 h -1 .
  • a molybdenum nickel catalyst is selected as the catalyst.
  • the sulfur content of the raw material FCC gasoline before the system treatment is 120 ppm, and the sulfur content of the FCC gasoline after the system treatment drops to 20 ppm.
  • the standard volume ratio of hydrogen to residual oil in the first micro-interface generator is 0.3:1; the standard volume ratio of hydrogen to residual oil in the second micro-interface generator is 700:1.
  • the air pressure inside the fluidized bed reactor 4 is controlled at 7 MPa, the reaction temperature is controlled at 200° C., and the space velocity is controlled at 0.7 h -1 .
  • the catalyst in the step 7 is a carbon-supported iron-based catalyst.
  • the reaction medium before and after the operation of the system was tested.
  • the test results are as follows:
  • the sulfur content in the raw material residue is 120 ppm, which is reduced to 25 ppm after the process of this hydrodesulfurization reaction process.
  • Hydrodesulfurization of coal tar is carried out using the above method and the system in the first embodiment of the system, wherein:
  • the standard volume ratio of hydrogen to coal tar in the first micro-interface generator is 0.4:1; the standard volume ratio of hydrogen to coal tar in the second micro-interface generator is 900:1.
  • the air pressure inside the fluidized bed reactor 4 is controlled at 10 MPa, the reaction temperature is controlled at 300° C., and the space velocity is controlled at 1 h -1 .
  • the catalyst in step 7 is a molybdenum cobalt catalyst.
  • the sulfur content in the raw coal tar is 120 ppm, which is reduced to 26 ppm after the process of this hydrodesulfurization reaction process.
  • the standard volume ratio of hydrogen to mixed oil in the first micro-interface generator is 0.3:1; the standard volume ratio of hydrogen to mixed oil in the second micro-interface generator is 800:1.
  • the air pressure inside the fluidized bed reactor 4 is controlled at 9 MPa, the reaction temperature is controlled at 250° C., and the space velocity is controlled at 1.5 h -1 .
  • the catalyst in the step 7 is an iron-cobalt catalyst.
  • the reaction medium before and after the operation of the system was tested.
  • the test results are as follows:
  • the sulfur content in the raw coal tar is 120 ppm, which is reduced to 23 ppm after the process of this hydrodesulfurization reaction process.
  • reaction system of the present invention can effectively remove sulfur in the reaction medium under a medium, low pressure and low temperature environment.

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Abstract

Un système d'hydrogénation à lit fluidisé de renforcement à micro-interface, comprenant : une unité d'alimentation en phase liquide (1), une unité d'alimentation en phase gazeuse (2), un générateur à micro-interface (3), un réacteur à lit fluidisé (4), et un réservoir de séparation (5).
PCT/CN2019/090280 2019-03-15 2019-06-06 Système d'hydrogénation à lit fluidisé de renforcement à micro-interface WO2020186637A1 (fr)

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CN114409502B (zh) * 2020-10-09 2024-07-16 中石化南京化工研究院有限公司 癸二酸二甲酯加氢制1,10-癸二醇低氢酯比合成工艺
CN114870756A (zh) * 2022-05-19 2022-08-09 江苏扬农化工集团有限公司 一种连续加氢制备1,3-丙二醇的方法和沸腾床反应器
CN115093880B (zh) * 2022-07-31 2024-03-19 中国石油化工股份有限公司 一种混合气泡流沸腾床渣油加氢工艺及装置

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