CN114100528A - Lower-feeding hydrogenation reactor and liquid-phase hydrogenation method - Google Patents

Lower-feeding hydrogenation reactor and liquid-phase hydrogenation method Download PDF

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CN114100528A
CN114100528A CN202010907013.2A CN202010907013A CN114100528A CN 114100528 A CN114100528 A CN 114100528A CN 202010907013 A CN202010907013 A CN 202010907013A CN 114100528 A CN114100528 A CN 114100528A
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gas
liquid
hydrogenation
reaction
reaction zone
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张方方
刘凯祥
张旭
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Sinopec Engineering Inc
Sinopec Engineering Group Co Ltd
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Sinopec Engineering Inc
Sinopec Engineering Group Co Ltd
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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
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
    • 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
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/0292—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds with stationary packing material in the bed, e.g. bricks, wire rings, baffles
    • 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
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
    • B01J8/0492—Feeding reactive fluids
    • 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
    • C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
    • C10G49/002—Apparatus for fixed bed hydrotreatment 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00823—Mixing elements
    • B01J2208/00831—Stationary elements
    • B01J2208/00849—Stationary elements outside the bed, e.g. baffles
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00938—Flow distribution elements

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention relates to the technical field of oil refining chemical industry, and discloses a lower feeding hydrogenation reactor and a liquid phase hydrogenation method, wherein the reactor comprises a shell, a hydrogenation reaction zone and a gas-liquid phase separation zone are arranged in the shell, the hydrogenation reaction zone comprises an axial reaction zone and/or a radial reaction zone, the axial reaction zone comprises a plurality of axial catalyst bed layers, the radial reaction zone comprises a plurality of radial catalyst bed layers, a gas distributor is arranged below the hydrogenation reaction zone and between the optional axial reaction zone and the radial reaction zone, the gas-liquid phase separation zone is positioned above the hydrogenation reaction zone, and a gas-liquid separation assembly is arranged in the gas-liquid phase separation zone; the gas-liquid separation assembly comprises an annular liquid accumulation plate, a reaction product channel and a flow guide piece which are coaxially arranged, a gas-liquid separation space is enclosed by the gas-liquid separation assembly and the shell positioned above the annular liquid accumulation plate, and the gas-liquid separation channel is formed inside the reaction product channel. The device and the method have the advantages of strong raw material adaptability, low energy consumption, low bed pressure drop, and low equipment investment and operation cost.

Description

Lower-feeding hydrogenation reactor and liquid-phase hydrogenation method
Technical Field
The invention relates to the technical field of oil refining chemical industry, in particular to a lower feeding hydrogenation reactor and a liquid phase hydrogenation method.
Background
The hydrogenation process is widely applied to the fields of petroleum refining, coal chemical industry, fine chemical industry and the like. In the petroleum refining industry, hydrocracking and hydrofining technologies are common, and a fixed bed hydrogenation reactor is usually used to reduce the size of raw oil molecules or remove impurities such as oxygen, nitrogen, sulfur, metals and the like in raw oil, and realize olefin saturation and partial aromatic saturation so as to improve the quality of oil products; in coal chemical industry, coal is mainly hydrogenated directly or indirectly to prepare liquid fuel or chemical products; in fine chemical industry, various organic products are prepared, such as hydrogenation of naphthalene to prepare tetrahydronaphthalene or decahydronaphthalene, hydrogenation of benzene to prepare cyclohexane, and the like.
In the prior art, in order to control the reaction temperature of a bed layer and avoid the deactivation of carbon deposition of a catalyst caused by the occurrence of a hydrogen-poor environment, a high hydrogen-oil ratio is generally adopted, after reaction products leave a reactor, a large amount of surplus hydrogen needs to be provided with systems such as amine liquid desulfurization, membrane recovery, PSA (pressure swing adsorption) and the like, and the recovered recycle hydrogen and new hydrogen are used as reaction raw materials together. The hydrogenation process usually uses fixed bed hydrogenation, and gas, liquid and solid phases generally exist in a reactor. The gas phase is the gasified raw oil and hydrogen, the liquid phase is the unvaporized raw oil, and the solid phase is the catalyst. Generally speaking, the volume ratio of hydrogen to oil in the hydrogenation reaction is 20: 1-5000: 1, hydrogen is a continuous phase, a liquid phase is a dispersed phase, and the hydrogen needs to be transferred from a gas phase main body to a liquid film, the liquid film to the diffusion of a catalyst active center and the hydrogenation reaction. If the hydrogen can be fully dissolved in the liquid phase, the consumption of the hydrogen can be greatly reduced, and devices such as a hydrogen circulating system, a circulating hydrogen compressor and the like, pipelines and the like are omitted, so that the equipment investment and the operating cost are reduced, and the occupied area can be reduced.
The reaction rate for removing impurities in the hydrogenation reaction is not only related to the concentration of the impurities, but also has close relationship with whether the active sites of the catalyst are fully wetted and the competitive reaction among the impurity reactions. The main factors influencing the catalyst wetting are the speed of the liquid phase flow velocity and the ratio of the gas phase flow velocity to the liquid phase flow velocity. It is generally believed that the liquid phase flow rate increases and the catalyst wetting effect increases, which in turn reduces the lubricating effect of the liquid phase feedstock on the catalyst due to the large hydrogen-to-oil ratio in conventional hydrogenation processes.
Patent document CN201811200084.8 discloses a method for combining an inferior hydrocarbon hydrocracking reaction section and a post-hydrofining reaction section, wherein the volume ratio of hydrogen to raw oil is 300: 1-4000: 1; patent document CN201710426072.6 discloses a method for increasing the reflux power of a liquid phase product of a gas-liquid material upflow hydrogenation reactor, wherein the volume ratio of hydrogen to raw oil is 50-5000; patent document CN201910645882.X discloses a hydrogenation combination method for treating residual oil and sludge pyrolysis oil, wherein the volume ratio of hydrogen to raw oil is 500-2000. The above patent documents have a common feature that hydrogen oil has a relatively high volume and a hydrogen gas circulation system and a recycle hydrogen compressor are required.
Patent documents US6428686B1, CN201910768245.1, CN201910170370.2, CN201920286166.2, CN201910170362.8, CN201920286167.7 and the like disclose a hydrogenation process in which hydrogen is dissolved in advance in a reaction feed, and the control of the hydrogenation reaction is achieved by controlling the flow rate of a reaction raw material by controlling the injection of the hydrogen amount. The above patent documents all have the disadvantages of large reaction pressure drop, long process flow, high equipment investment, large occupied area and the like.
In the existing hydrogenation reaction process, the gasification raw oil needs to consume more energy, the use of a compressor to compress hydrogen not only has high energy consumption, but also needs to occupy larger space, the compression of hydrogen also needs to consume more energy, and the hydrogenation reaction temperature is high.
Disclosure of Invention
In view of the problems existing in the prior hydrogenation process, the inventor of the invention finds out a hydrogenation reactor and a liquid phase hydrogenation method with practical value through repeated research, experiments, engineering design and construction, and solves the defects of high energy consumption, high production cost, large occupied area and the like in the prior hydrogenation technology.
The invention provides a lower feeding hydrogenation reactor, which comprises a shell, wherein the bottom of the shell is provided with a feeding pipeline, the top of the shell is provided with a gas phase outlet pipeline, and the upper part of the shell is provided with a liquid phase outlet pipeline;
a hydrogenation reaction zone and a gas-liquid phase separation zone are arranged in the shell, the hydrogenation reaction zone comprises an axial reaction zone and/or a radial reaction zone, the axial reaction zone is composed of a plurality of axial catalyst bed layers, the radial reaction zone is composed of a plurality of radial catalyst bed layers, gas distributors are arranged below the hydrogenation reaction zone and between the optional axial reaction zone and the radial reaction zone, the gas-liquid phase separation zone is positioned above the hydrogenation reaction zone, and a gas-liquid separation assembly is arranged in the gas-liquid phase separation zone;
the gas-liquid separation subassembly includes annular hydrops board, reaction product passageway and the water conservancy diversion spare of coaxial setting, the outer fringe of annular hydrops board links to each other with shells inner wall, the lower extreme of reaction product passageway with the inner edge of annular hydrops board links to each other, the water conservancy diversion spare is the top seal, the open section of thick bamboo in bottom, the water conservancy diversion spare covers and establishes in reaction product passageway top, the value scope of annular hydrops board and horizontal plane contained angle alpha is: alpha is more than or equal to 0 degree and less than or equal to 75 degrees;
the gas-liquid separation assembly and the shell positioned above the annular liquid accumulation plate enclose a gas-liquid separation space, a gas-liquid separation channel is formed inside the reaction product channel, and the liquid phase outlet pipeline is communicated with the lower part of the gas-liquid separation space.
A second aspect of the invention provides a liquid phase hydrogenation process employing a lower feed hydrogenation reactor, the liquid phase hydrogenation process comprising the steps of:
(1) mixing raw oil with hydrogen to obtain hydrogen-mixed raw oil, wherein the molar ratio of the hydrogen to the raw oil is 0.01: 99.9-30: 1;
(2) and (3) feeding the hydrogen-mixed raw oil into the lower feeding hydrogenation reactor to carry out raw oil hydrogenation reaction, and carrying out gas-liquid separation on the reaction product through a gas-liquid separation component to obtain a gas-phase product and a liquid-phase product.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the lower feeding hydrogenation reactor and the liquid phase hydrogenation method provided by the invention, the molar ratio of hydrogen to raw oil is 0.01: 99.9-30: 1; the hydrogen consumption is less, the reaction feeding is in a gas-liquid mixed state, the liquid phase is a continuous phase, and the gas phase is a dispersed phase, so that the hydrogenation reaction is a gas-liquid reaction, the high temperature is not needed, and the energy consumption required by the hydrogenation reaction is reduced; the gas distributor is arranged in the upflow reactor to realize the sufficient mixing of the hydrogen and the raw oil, and the gas-liquid separation component is used for realizing the primary gas-liquid separation of the product; in addition, the hydrogen consumption is less, and a compressor is not required to compress the hydrogen and recycle the hydrogen, so that the liquid phase hydrogenation method provided by the invention has low energy consumption and low equipment investment.
2. In the invention, the hydrogenation reaction zone adopts the combination of an axial catalyst bed layer and a radial catalyst bed layer, and the catalysts in the two bed layers can be selectively filled with the same or different catalysts according to actual requirements. The axial direction and the radial catalyst bed layer are combined, so that not only can the gas-liquid phase flow uniformly be realized, the flow dead zone can be avoided, but also the pressure of the hydrogenation reaction zone is reduced. In addition, the guide plate is arranged in the axial catalyst bed layer, so that a hydrogen-poor environment can be avoided, and the nonuniformity of artificially filled catalyst is eliminated.
3. In the invention, as the gas-liquid separation area is provided with the flow guide assembly, not only can the reaction product be prevented from directly entering a top gas phase outlet pipeline after flowing out from a top outlet of the reaction product channel, but also the buffer effect can be achieved, the liquid carried by the gas phase is reduced, and the effective gas-liquid separation is realized.
4. In the invention, as liquid-phase hydrogenation is adopted, a large amount of hydrogen is pre-dissolved in the liquid-phase raw material, the hydrogenation reaction temperature is lower, the operation severity of a reactor, a heat exchanger and related pipelines is reduced, the investment and the operation energy consumption are obviously reduced, and by accelerating the mass transfer rate of a gas-liquid phase, the removal rate of impurities such as sulfur, nitrogen, metal and the like is high, the reactor severity is low, and the service life of the catalyst and the operation period of the device are prolonged.
5. In the invention, the number of the axial and radial catalyst beds can be selected according to the actual hydrogenation reaction system, and the hydrogenation reactors can be arranged in series or in parallel, so that the impurity removal rate is increased, and the flexibility and the processing capacity of the device are improved.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention.
FIG. 1 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 1 of this invention.
FIG. 2 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 4 of this invention.
FIG. 3 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 5 of this invention.
FIG. 4 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 6 of this invention.
FIG. 5 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 7 of this invention.
FIG. 6 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 8 of this invention.
FIG. 7 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 9 of this invention.
FIG. 8 is a schematic diagram of the structure of a lower feed hydrogenation reactor in example 10 of this invention.
FIG. 9 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 11 of this invention.
FIG. 10 is a schematic diagram of the structure of a lower feed hydrogenation reactor of example 12 of this invention.
Fig. 11 is a schematic structural view of a flow guide member in embodiment 1 of the present invention.
Fig. 12 is a schematic structural view of a flow guide member in embodiment 6 of the present invention.
Description of the reference numerals
1-a feed line, 2-a gas phase outlet line, 3-a liquid phase outlet line, 4-a hydrogen inlet line;
101-a housing;
201-a gas distributor, 202-an axial catalyst bed layer, 203-an annular liquid accumulation plate, 204-an upper cover plate, 205-a reaction product channel, 206-a radial catalyst bed layer, 207-a flow guide piece, 208-a flow guide strip seam, 209-a flow guide hole, 210-a gas-liquid separation component, 211-a vertical through hole, 212-a lower cover plate, 213-an annular gap and 214-a flow guide plate.
Detailed Description
In order that the present invention may be more readily understood, the following detailed description of the invention is given with reference to the accompanying drawings and embodiments, which are given by way of illustration only and are not intended to limit the invention.
According to a first aspect of the invention, the invention provides a lower feeding hydrogenation reactor, which comprises a shell, wherein the bottom of the shell is provided with a feeding pipeline, the top of the shell is provided with a gas phase outlet pipeline, and the upper part of the shell is provided with a liquid phase outlet pipeline;
a hydrogenation reaction zone and a gas-liquid phase separation zone are arranged in the shell, the hydrogenation reaction zone comprises an axial reaction zone and/or a radial reaction zone, the axial reaction zone is composed of a plurality of axial catalyst bed layers, the radial reaction zone is composed of a plurality of radial catalyst bed layers, gas distributors are arranged below the hydrogenation reaction zone and between the optional axial reaction zone and the radial reaction zone, the gas-liquid phase separation zone is positioned above the hydrogenation reaction zone, and a gas-liquid separation assembly is arranged in the gas-liquid phase separation zone;
the gas-liquid separation subassembly includes annular hydrops board, reaction product passageway and the water conservancy diversion spare of coaxial setting, the outer fringe of annular hydrops board links to each other with shells inner wall, the lower extreme of reaction product passageway with the inner edge of annular hydrops board links to each other, the water conservancy diversion spare is the top seal, the open section of thick bamboo in bottom, the water conservancy diversion spare covers and establishes in reaction product passageway top, the value scope of annular hydrops board and horizontal plane contained angle alpha is: alpha is more than or equal to 0 degree and less than or equal to 75 degrees;
the gas-liquid separation assembly and the shell positioned above the annular liquid accumulation plate enclose a gas-liquid separation space, a gas-liquid separation channel is formed inside the reaction product channel, and the liquid phase outlet pipeline is communicated with the lower part of the gas-liquid separation space.
Preferably, a guide plate is arranged in the axial catalyst bed layer, and the guide plate can fix the catalyst to prevent the catalyst from moving up and down or left and right, and can ensure that gas-liquid material flows smoothly in the upflow reactor to eliminate the nonuniformity of artificially filled catalyst. In the invention, the flow guide plate can be at least one selected from a grating plate, a silk screen, an opening plate and a slit plate. The material of the guide plate can be the same as or better than that of the reactor shell. According to the invention, the included angle between the guide plate and the horizontal plane is 0-90 degrees.
According to the invention, in order to realize low pressure drop and reaction performance, the hydrogenation reaction zone is provided with a radial reaction zone, preferably, the top of the radial catalyst bed layer is provided with an upper cover plate, the bottom of the radial catalyst bed layer is provided with a lower cover plate, the center of the radial catalyst bed layer is provided with a vertical through hole, an annular gap is arranged between the outer side wall of the radial catalyst bed layer and the inner side wall of the shell, the diameter of the lower cover plate is the same as the outer diameter of the radial catalyst bed layer, the center of the upper cover plate is provided with a hole with the same diameter as the vertical through hole of the radial catalyst bed layer, and the outer edge of the upper cover plate is connected with the shell. The upper cover plate and the lower cover plate ensure that reaction feeding only enters from the annular space and is uniformly distributed on the radial catalyst bed layer, and after the radial catalyst bed layer reacts, products are collected in the vertical through hole and leave the radial reaction zone from the upper part of the vertical through hole. Radial catalyst bed arrangements are well known to those skilled in the art and the present invention will not be described in detail herein.
According to the invention, in order to avoid that a reaction product directly enters a top gas phase outlet pipeline after flowing out from a top outlet of a reaction product channel and realize effective separation of a gas phase and a liquid phase in a gas-liquid phase separation zone, a flow guide part is arranged above the reaction product channel, after the gas-liquid phase product flows out from a reaction product channel port, the gas-liquid phase reaction product flowing upwards returns back and flows downwards due to the blocking effect of the flow guide part, the liquid phase flows downwards under the dual action of inertia and gravity due to the sudden increase of the sectional area of a flow channel, and a gas phase substance in the liquid phase is separated out and flows upwards due to the flash evaporation effect, so that the gas-liquid phase separation is realized.
Preferably, the side wall of the flow guide piece is provided with flow guide strip seams and/or flow guide holes, and the aperture ratio of the side wall of the flow guide piece is 0-0.55;
the width of the diversion strip seam is 10 mm-150 mm, and the diameter of the diversion hole is 10 mm-200 mm.
According to the invention, the annular liquid accumulation plate and the horizontal plane form a certain included angle, so that a flow dead zone formed in the annular liquid accumulation plate can be avoided, a flow dead zone formed by upward flow of a gas-liquid phase product can be avoided, the upward flow uniformity of the gas-liquid phase product in a catalyst bed layer can be balanced, the stable operation of a reactor is facilitated, and the operation period is prolonged. Preferably, the value range of the included angle α between the annular liquid collecting plate and the horizontal plane is as follows: alpha is more than or equal to 0 degree and less than or equal to 60 degrees.
Preferably, the distance between the top of the flow guide piece and the upper end of the reaction product channel is 300-1500 mm, and the width of a horizontal annular gap formed by the inner side wall of the flow guide piece and the outer side wall of the reaction product channel is 0.05-0.3 time of the inner diameter of the shell.
Preferably, the bottom of the flow guide member is lower than the upper end of the reaction product channel, and the distance between the flow guide member and the reaction product channel is 100-2000 mm.
In order to control the discharge rate of the liquid-phase product in the upflow reactor, stabilize the reaction pressure, and prevent the cross-pressure of the liquid phase, the upflow reactor is further provided with a liquid level detecting element for detecting the liquid level in the gas-liquid separation space and a liquid level control valve. When the liquid level detection element detects that the liquid level in the gas-liquid separation space is higher than a first preset liquid level, the liquid level control valve is opened, and a liquid-phase product is discharged; and when the liquid level detection element detects that the liquid level in the gas-liquid separation space is higher than a second preset liquid level, the liquid level control valve is closed, liquid drainage is stopped, wherein the first preset liquid level is higher than the second preset liquid level.
In order to realize the uniform distribution of gas-liquid reaction feeding materials in a hydrogenation reaction zone and simultaneously achieve the aim of low reaction pressure drop, the axial catalyst bed layer and the radial catalyst bed layer are combined, and the number of layers of the axial catalyst bed layer and the radial catalyst bed layer can be 1-6, preferably 1-3. A gas distributor can be arranged below each catalyst bed layer. The axial catalyst bed and the radial catalyst bed can be filled with the same or different catalyst types.
According to the invention, the gas distributor can be used for injecting hydrogen into the catalyst bed layer through the gas distributor if a hydrogen-poor working condition occurs or injecting cold hydrogen into the catalyst bed layer through the gas distributor when working conditions such as temperature runaway of the catalyst bed layer occur so as to reduce the temperature of the catalyst bed layer. The arrangement of the gas distributor increases the operational flexibility of the device on the one hand and also improves the safety performance of the device on the other hand.
The lower feeding hydrogenation reactor is an up-flow reaction-separation combined type reactor, and the reactor has double functions of reaction and separation, so that the energy consumption, the operation cost and the construction cost of a hydrogenation device are greatly reduced. Two or more lower feeding hydrogenation reactors can be arranged in series or in parallel according to actual conditions. For example, in the area with limited equipment transportation, if the series of reactors has a larger size, such as 6m inner diameter, two lower feeding hydrogenation reactors with the same size can be arranged in parallel, so that the processing capacity of the device can be increased to a certain extent, and the operation flexibility of the device is increased.
According to a second aspect of the present invention, the present invention provides a liquid phase hydrogenation process employing a lower feed hydrogenation reactor, the liquid phase hydrogenation process comprising the steps of:
(1) mixing raw oil with hydrogen to obtain hydrogen-mixed raw oil, wherein the molar ratio of the hydrogen to the raw oil is 0.01: 99.9-30: 1;
(2) and (3) feeding the hydrogen-mixed raw oil into the lower feeding hydrogenation reactor to carry out raw oil hydrogenation reaction, and carrying out gas-liquid separation on the reaction product through a gas-liquid separation component to obtain a gas-phase product and a liquid-phase product.
In the invention, the raw oil can be at least one of naphtha, gasoline, pyrolysis gasoline, aviation kerosene, diesel oil, wax oil, residual oil, coal tar, catalytic slurry oil and deoiled asphalt.
In order to conveniently control the hydrogenation reaction process, reduce the non-chemical hydrogen consumption and reduce the equipment and pipeline sizes so as to achieve the purposes of reducing the investment and the operation energy consumption, the liquid hourly space velocity of the raw oil can be 0.02-30 h-1Preferably 0.05～20h-1. Preferably, the molar ratio of the hydrogen to the raw oil is 0.03: 99.7-15: 1.
In the reaction process of the invention, the reaction feed is in a gas-liquid mixed state, i.e. the raw oil is in a gas-liquid mixed phase, and a person skilled in the art can set the reaction temperature and the reaction pressure of the hydrogenation reaction according to the gas-liquid mixed state. In consideration of the energy consumed by the reaction and the reaction efficiency, the reaction temperature of the raw oil hydrogenation reaction is 100-460 ℃, and the reaction pressure is 0.5-25.0 MPaG. Preferably, the reaction temperature of the raw oil hydrogenation reaction is 150-430 ℃, the reaction pressure is 0.9-20.0 MPaG, and the impurity removal rate is high at the reaction temperature and the reaction pressure.
According to the invention, the components, shapes and sizes of the catalysts in the axial catalyst bed layer and the radial catalyst bed layer are not particularly limited as long as the impurities such as sulfur, nitrogen, arsenic, lead and the like in the raw oil can be removed.
The process parameters which are not limited in the invention can be selected conventionally according to the prior art.
The present invention will be described in detail by way of examples.
Examples 1-12 illustrate a lower feed hydrogenation reactor and a liquid phase hydrogenation process according to the present invention.
Example 1
As shown in fig. 1 and fig. 11, the lower feeding hydrogenation reactor comprises a shell 101, wherein a feeding pipeline 1 is arranged at the bottom of the shell 101, a gas phase outlet pipeline 2 is arranged at the top of the shell 101, and a liquid phase outlet pipeline 3 is arranged at the upper part of the shell;
a hydrogenation reaction zone and a gas-liquid phase separation zone are arranged in the shell 101, the hydrogenation reaction zone comprises an axial reaction zone and a radial reaction zone, the axial reaction zone is formed by a layer of axial catalyst bed layer 202, the radial reaction zone is formed by a layer of radial catalyst bed layer 206, the axial catalyst bed layer 202 is arranged below the radial catalyst bed layer 206, a gas distributor 201 is arranged below the axial catalyst bed layer 202, the gas distributor 201 is connected with a hydrogen inlet pipeline 4, the gas-liquid phase separation zone is positioned above the hydrogenation reaction zone, and a gas-liquid separation component 210 is arranged in the gas-liquid phase separation zone;
the gas-liquid separation assembly comprises an annular liquid accumulation plate 203, a reaction product channel 205 and a flow guide part 207 which are coaxially arranged, the outer edge of the annular liquid accumulation plate 203 is connected with the inner wall of the shell 101, the lower end of the reaction product channel 205 is connected with the inner edge of the annular liquid accumulation plate 203, the flow guide part 207 is a cylinder with a sealed top and an open bottom, the flow guide part 207 covers the reaction product channel 205, and the included angle alpha between the annular liquid accumulation plate 203 and the horizontal plane takes a value of 45 degrees;
the gas-liquid separation module 210 and the housing 101 above the annular liquid accumulation plate 203 enclose a gas-liquid separation space, a gas-liquid separation channel is formed inside the reaction product channel 205, and the liquid phase outlet pipeline 3 is communicated with the lower part of the gas-liquid separation space.
The top of the radial catalyst bed layer 206 is provided with an upper cover plate 204, the bottom of the radial catalyst bed layer is provided with a lower cover plate 212, the center of the radial catalyst bed layer 206 is provided with a vertical through hole 211, an annular gap 213 is arranged between the outer side wall of the radial catalyst bed layer 206 and the inner side wall of the shell 101, the diameter of the lower cover plate 212 is the same as the outer diameter of the radial catalyst bed layer 206, the center of the upper cover plate 204 is provided with a hole with the same diameter as the vertical through hole 211 of the radial catalyst bed layer 206, and the outer edge of the upper cover plate 204 is connected with the shell 101.
The side wall of the flow guide piece 207 is provided with a flow guide strip slit 208, and the opening ratio of the side wall of the flow guide piece 207 is 0.2; the width of the flow guide strip slit 208 is 25 mm.
The distance between the top of the flow guide 207 and the upper end of the reaction product channel 205 was 550mm, and the width of the horizontal annular gap formed between the inner side wall of the flow guide 207 and the outer side wall of the reaction product channel 205 was 0.08 times the inner diameter of the housing. The bottom of the flow guide 207 is lower than the upper end of the reaction product channel 205, and the distance between the two is 250 mm.
The lower feed hydrogenation reactor was used for naphtha hydrogenation, naphtha was a mixture of straight run naphtha and hydrocracked heavy naphtha, and the mixture was fed as a unit, and the composition of the mixture is shown in table 1. The hydrogenation method comprises the following steps:
(1) mixing naphtha with hydrogen to obtain hydrogen-mixed naphtha, wherein the molar ratio of the hydrogen to the naphtha is 0.05: 1;
(2) and (3) feeding the mixed hydrogen naphtha into the lower feeding hydrogenation reactor for naphtha hydrogenation reaction, and performing gas-liquid separation on the reaction product through a gas-liquid separation component 210 to obtain a gas-phase product and a liquid-phase product.
The liquid hourly space velocity of the naphtha is 6h-1The reaction temperature of the naphtha hydrogenation reaction is 210 ℃, and the reaction pressure is 2.0 MPaG. The same catalyst is filled in the axial catalyst bed layer and the radial catalyst bed layer, and is a Co-Mo type hydrogenation catalyst, the impurities such as sulfur, nitrogen, metal and the like are removed by hydrofining reaction, reaction products with the impurities removed are generated, and the gas-phase product and the liquid-phase product are respectively sent to downstream processing.
The detection shows that the contents of sulfur and nitrogen in the hydrogenation product are less than 0.4ppm, the content of arsenic is less than 0.8ppb, the content of lead is less than 10ppb, and the pressure drop of a bed layer is 20 kPa.
TABLE 1
Categories Straight run naphtha Hydrocracking of heavy naphtha
Distillation range/. degree.C 34.5～165 83～178
S，ppm 190 0.55
N，ppm 3.4 0.6
As，ppb 3.5 1.1
Pb，ppb 4.1 20
Cu+，ppb 20 25
Bromine per kg oil, mg 190 9
Example 2
The difference from example 1 is that: the molar ratio of hydrogen to naphtha is 0.038: 1, and the liquid hourly space velocity of naphtha is 4.2h-1The reaction temperature of naphtha hydrogenation was 205 ℃ and the reaction pressure was 2.05 MPaG.
The detection shows that the contents of sulfur and nitrogen in the hydrogenation product are less than 0.3ppm, the content of arsenic is less than 0.8ppb, the content of lead is less than 6.5ppb, and the pressure drop of a bed layer is 15 kPa.
Example 3
The difference from example 1 is that: the molar ratio of hydrogen to naphtha is 0.03: 1, and the liquid hourly space velocity of naphtha is 5h-1The reaction temperature of the naphtha hydrogenation reaction was 198 ℃ and the reaction pressure was 2.1 MPaG.
The detection shows that the contents of sulfur and nitrogen in the hydrogenation product are less than 0.35ppm, the content of arsenic is less than 0.9ppb, the content of lead is less than 8ppb, and the pressure drop of a bed layer is 17 kPa.
Example 4
As shown in fig. 2, the difference from embodiment 1 is that: the radial catalyst bed 206 is disposed below the axial catalyst bed 202.
Example 5
As shown in fig. 3, the difference from embodiment 1 is that: a gas distributor 201 is additionally arranged between the radial catalyst bed layer 206 and the axial catalyst bed layer 202, and the gas distributor 201 is connected with a hydrogen inlet pipeline 4.
The lower feeding hydrogenation reactor of the embodiment is applied to diesel hydrogenation, wherein the axial catalyst bed layer is filled with a Mo-Co catalyst, and the radial catalyst bed layer is filled with a Mo-Ni catalyst. The reaction temperature is 355 ℃, the pressure is 9.0MPaG, and the liquid hourly space velocity of the diesel oil is 2.8h-1The molar ratio of hydrogen to diesel oil is 0.8: 1. In the embodiment, the total sulfur at the diesel inlet is 0.85 wt%, and the sulfur content of the diesel at the top liquid phase outlet is not more than 10 mug/g.
By arranging the gas distributor 201 between the radial catalyst bed 206 and the axial catalyst bed 202 and below the axial catalyst bed 202, when the catalyst bed has temperature runaway or needs emergency stop and other working conditions, cold hydrogen can be injected into the catalyst bed through the gas distributor 201, so that the bed temperature is reduced. The provision of the gas distributor 201 increases the operational flexibility of the device on the one hand and also the safety of the device on the other hand.
Example 6
As shown in fig. 4 and 12, the present embodiment is different from embodiment 1 in that: the included angle alpha between the annular liquid accumulation plate 203 and the horizontal plane is 0 degree, the side wall of the flow guide piece 207 is provided with a flow guide hole 209, and the aperture ratio of the side wall of the flow guide piece 207 is 0.2; the diameter of the diversion hole is 25 mm. The process parameters of this example were the same as example 1. The same effect as in example 1 was obtained by the same procedure as in example 1.
Example 7
As shown in fig. 5, the difference from embodiment 1 is that: a horizontal guide plate 214 is additionally arranged in the axial catalyst bed layer 202, and the guide plate 214 is a wire mesh.
Example 8
As shown in fig. 6, the difference from embodiment 4 is that: a horizontal guide plate 214 is additionally arranged in the axial catalyst bed layer 202, and the guide plate 214 is a wire mesh.
Example 9
As shown in fig. 7, the difference from embodiment 5 is that: a vertical guide plate 214 is additionally arranged in the axial catalyst bed layer 202, and the guide plate 214 is a wire mesh.
In this example, the diesel hydrogenation was also used, and the reaction conditions were the same as in example 5. After hydrogenation reaction, the sulfur content of the diesel oil at the top liquid phase outlet is not more than 10 mug/g. As the guide plate 214 is additionally arranged, the temperature deviation of the catalyst bed layer is less than 0.5 ℃ through long-period experiment comparison, which shows that the guide plate is beneficial to the uniform distribution of gas-liquid reactants in the catalyst bed layer.
Example 10
As shown in fig. 8, the difference from embodiment 5 is that: the guide plate 214 is additionally arranged in the axial catalyst bed layer 202, the guide plate 214 is a grid plate, and an included angle of 45 degrees is formed between the guide plate 214 and the horizontal plane.
In this example, the diesel hydrogenation was also used, and the reaction conditions were the same as in example 5. After hydrogenation reaction, the sulfur content of the diesel oil at the top liquid phase outlet is not more than 10 mug/g. As the guide plate 214 is additionally arranged, the temperature deviation of the catalyst bed layer is less than 0.5 ℃ through long-period experiment comparison, which shows that the guide plate is beneficial to the uniform distribution of gas-liquid reactants in the catalyst bed layer.
Example 11
As shown in fig. 9, the lower feeding hydrogenation reactor of the present embodiment includes a shell 101, a feeding pipeline 1 is disposed at the bottom of the shell 101, a gas phase outlet pipeline 2 is disposed at the top, and a liquid phase outlet pipeline 3 is disposed at the upper part of the shell 101; an axial catalyst bed layer 202 is arranged in the shell 101, a gas distributor 201 is arranged at the lower part of the axial catalyst bed layer 202, a hydrogen inlet pipeline 4 is connected to the gas distributor 201, a horizontal guide plate 214 is arranged in the axial catalyst bed layer 202, the guide plate 214 is a wire mesh, and the gas-liquid separation assembly 210 is the same as that in the embodiment 1.
In this example, the diesel hydrogenation was used and the reaction conditions were the same as in example 5. After hydrogenation reaction, the sulfur content of the diesel oil at the top liquid phase outlet is not more than 10 mug/g. As the guide plate 214 is additionally arranged, the temperature deviation of the catalyst bed layer is less than 0.6 ℃ through long-period experiment comparison, which shows that the guide plate is beneficial to the uniform distribution of gas-liquid reactants in the catalyst bed layer.
Example 12
As shown in fig. 10, the lower feeding hydrogenation reactor of the present embodiment includes a shell 101, a feeding pipeline 1 is provided at the bottom of the shell 101, a gas phase outlet pipeline 2 is provided at the top, and a liquid phase outlet pipeline 3 is provided at the upper part; a radial catalyst bed layer 206 is arranged in the shell 101, a gas distributor 201 is arranged at the lower part of the radial catalyst bed layer 206, a hydrogen inlet pipeline 4 is connected to the gas distributor 201, and the gas-liquid separation assembly 210 and the radial catalyst bed layer 206 are the same as those in the embodiment 1.
The lower feed hydrogenation reactor of this example was used for residue hydrogenation. The raw oil is the mixture of normal pressure residual oil and vacuum residual oil according to the mass ratio of 52 percent to 48 percent. The raw oil comprises, by weight, 3.8% of total sulfur, 0.35% of total nitrogen, 13.6% of residual carbon, 0.012% of heavy metal, and 0.998g/cm of raw oil density at 20 deg.C3Viscosity at 100 ℃ of 164mm2.s-1。
The reaction temperature is 370 ℃, the pressure is 19.5MPaG, and the liquid hourly space velocity of the raw oil is 0.75h-1The molar ratio of hydrogen to raw oil is 4.2: 1. The catalyst adopts Ni-Co-Mo as an active component and a butterfly catalyst. After hydrogenation reaction, the total sulfur content, the total nitrogen content and the heavy metal content of the product are respectively reduced by 65 percent, 38 percent and 73 percent. The bed pressure drop is 46 percent lower than that of the fixed bed axial reactor with the same treatment scale.
Comparative example
The hydrogen is compressed to 2.4MPaG by a compressor, mixed with naphtha according to the mol ratio of 3.1: 1, and the mixed hydrogen and naphtha are heated to 320 ℃ by a heating furnace to form reaction feeding, and the reaction feeding is gaseous at the temperature.
Feeding the reaction feed into a fixed bed reactor, feeding the reaction feed into a catalyst bed layer to carry out naphtha hydrofining reaction, wherein the reaction temperature is 325 ℃, the reaction pressure is 2.3MPaG, and the liquid phase of the reaction feed isThe space velocity is 4.4h-1To produce a hydrogenated naphtha product without impurities.
The detection shows that the content of sulfur and nitrogen in the hydrogenated naphtha product is 3.1ppm and 4.5ppm respectively, the content of arsenic is 1.0ppb, and the content of lead is 17 ppb.
The comparison shows that under the condition of reducing the reaction temperature and the hydrogen-oil ratio, namely under the condition of reducing the energy consumption and the cost, the contents of sulfur, nitrogen and metal impurities in the hydrogenation product are lower than those of a comparative example, so that the lower feeding reactor and the hydrogenation method have low energy consumption and cost and the hydrogenation product has better quality.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.

Claims (10)

1. A lower feeding hydrogenation reactor is characterized by comprising a shell, wherein the bottom of the shell is provided with a feeding pipeline, the top of the shell is provided with a gas phase outlet pipeline, and the upper part of the shell is provided with a liquid phase outlet pipeline;
a hydrogenation reaction zone and a gas-liquid phase separation zone are arranged in the shell, the hydrogenation reaction zone comprises an axial reaction zone and/or a radial reaction zone, the axial reaction zone is composed of a plurality of axial catalyst bed layers, the radial reaction zone is composed of a plurality of radial catalyst bed layers, gas distributors are arranged below the hydrogenation reaction zone and between the optional axial reaction zone and the radial reaction zone, the gas-liquid phase separation zone is positioned above the hydrogenation reaction zone, and a gas-liquid separation assembly is arranged in the gas-liquid phase separation zone;
the gas-liquid separation subassembly includes annular hydrops board, reaction product passageway and the water conservancy diversion spare of coaxial setting, the outer fringe of annular hydrops board links to each other with shells inner wall, the lower extreme of reaction product passageway with the inner edge of annular hydrops board links to each other, the water conservancy diversion spare is the top seal, the open section of thick bamboo in bottom, the water conservancy diversion spare covers and establishes in reaction product passageway top, the value scope of annular hydrops board and horizontal plane contained angle alpha is: alpha is more than or equal to 0 degree and less than or equal to 75 degrees;
the gas-liquid separation assembly and the shell positioned above the annular liquid accumulation plate enclose a gas-liquid separation space, a gas-liquid separation channel is formed inside the reaction product channel, and the liquid phase outlet pipeline is communicated with the lower part of the gas-liquid separation space.
2. The lower feed hydrogenation reactor according to claim 1, wherein a deflector plate is disposed in the axial catalyst bed, the deflector plate being selected from at least one of a grid plate, a wire mesh, an apertured plate, and a slotted plate; the included angle between the guide plate and the horizontal plane is 0-90 degrees.
3. The lower feed hydrogenation reactor according to claim 1, wherein an upper cover plate is arranged at the top of the radial catalyst bed, a lower cover plate is arranged at the bottom of the radial catalyst bed, a vertical through hole is arranged at the center of the radial catalyst bed, an annular gap is arranged between the outer side wall of the radial catalyst bed and the inner side wall of the shell, the diameter of the lower cover plate is the same as the outer diameter of the radial catalyst bed, a hole with the same diameter as the vertical through hole of the radial catalyst bed is arranged at the center of the upper cover plate, and the outer edge of the upper cover plate is connected with the shell.
4. The lower feeding hydrogenation reactor according to claim 1, wherein the side wall of the flow guide piece is provided with flow guide strip seams and/or flow guide holes, and the opening ratio of the side wall of the flow guide piece is 0-0.55;
the width of the diversion strip seam is 10 mm-150 mm, and the diameter of the diversion hole is 10 mm-200 mm.
5. The lower feed hydrogenation reactor according to claim 1 or 4, wherein the angle α between the annular hydroplate and the horizontal plane is in the range of: alpha is more than or equal to 0 degree and less than or equal to 60 degrees;
the distance between the top of the flow guide piece and the upper end of the reaction product channel is 300-1500 mm, and the width of a horizontal annular gap formed by the inner side wall of the flow guide piece and the outer side wall of the reaction product channel is 0.05-0.3 time of the inner diameter of the shell; the bottom of the flow guide piece is lower than the upper end of the reaction product channel, and the distance between the flow guide piece and the reaction product channel is 100-2000 mm.
6. A liquid phase hydrogenation process employing the lower feed hydrogenation reactor of any of claims 1-5, characterized in that the liquid phase hydrogenation process comprises the steps of:
(1) mixing raw oil with hydrogen to obtain hydrogen-mixed raw oil, wherein the molar ratio of the hydrogen to the raw oil is 0.01: 99.9-30: 1;
(2) and (3) feeding the hydrogen-mixed raw oil into the lower feeding hydrogenation reactor to carry out raw oil hydrogenation reaction, and carrying out gas-liquid separation on the reaction product through a gas-liquid separation component to obtain a gas-phase product and a liquid-phase product.
7. The liquid-phase hydrogenation method according to claim 6, wherein the molar ratio of the hydrogen to the feedstock oil is 0.03: 99.7 to 15: 1.
8. The liquid-phase hydrogenation method according to claim 6, wherein the liquid hourly space velocity of the feedstock oil is 0.02-30 h-1；
The reaction temperature of the raw oil hydrogenation reaction is 100-460 ℃, and the reaction pressure is 0.5-25.0 MPaG.
9. The liquid-phase hydrogenation method according to claim 8, wherein the liquid hourly space velocity of the feedstock oil is 0.05-20 h-1；
The reaction temperature of the raw oil hydrogenation reaction is 150-430 ℃, and the reaction pressure is 0.9-20.0 MPaG.
10. The liquid-phase hydrogenation process of claim 6, wherein the feedstock oil is at least one of naphtha, gasoline, pyrolysis gasoline, aviation kerosene, diesel, wax oil, residual oil, coal tar, catalytic slurry oil, and deoiled asphalt.
CN202010907013.2A 2020-09-01 2020-09-01 Lower-feeding hydrogenation reactor and liquid-phase hydrogenation method Pending CN114100528A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103627427A (en) * 2012-08-22 2014-03-12 中国石油化工集团公司 Two-stage hydrogenation system, and hydrogenation method
CN103834433A (en) * 2012-11-21 2014-06-04 中国石油化工集团公司 Upstroke reaction separator and hydrogenation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103627427A (en) * 2012-08-22 2014-03-12 中国石油化工集团公司 Two-stage hydrogenation system, and hydrogenation method
CN103834433A (en) * 2012-11-21 2014-06-04 中国石油化工集团公司 Upstroke reaction separator and hydrogenation method

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