CN113877488B - Up-flow hydrogenation reaction device based on tubular microporous medium foaming mechanism - Google Patents
Up-flow hydrogenation reaction device based on tubular microporous medium foaming mechanism Download PDFInfo
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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
- B01J8/06—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 in tube reactors; the solid particles being arranged in tubes
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (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 provides an up-flow hydrogenation reaction device based on a tubular microporous medium foaming mechanism, which can carry out secondary bubbling on each stage of reaction product, realize quick dissolution of hydrogen, uniform distribution of gas and liquid, high-efficiency dispersion of hydrogen supplementing and reduction of hydrogen gradient, and comprises an outer cylinder, wherein the upper end of the outer cylinder is provided with an exhaust pipe, and the lower end of the outer cylinder is provided with a raw oil feed pipe; the inside of the outer cylinder body is provided with a plurality of tubular microporous foaming reactors through a supporting plate, the bottom of the outer cylinder body is provided with a hydrogen storage chamber and a liquid distributor, and the hydrogen storage chamber is communicated with the outside through an air inlet pipe on the side wall of the outer cylinder body to supply hydrogen and supply hydrogen into the tubular microporous foaming reactors; a gas-liquid separation channel is arranged above the tubular microporous foaming reactor, the bottom of the gas-liquid separation channel is connected with an annular partition plate, and the central hole of the annular partition plate protrudes upwards to form the gas-liquid separation channel; and a liquid discharge pipe is further arranged on the outer cylinder above the annular partition plate.
Description
Technical Field
The invention belongs to the technical field of clean production of low-hydrogen-consumption oil products, and particularly relates to the technical field of continuous liquid-phase hydrogenation reactions of low-hydrogen-consumption micro-bubbling series oil products in the petrochemical industry.
Background
In the fuel structures of all countries of the world, industrial grade oil products such as diesel oil, kerosene and the like have the characteristics of high efficiency and durability, and have a high proportion in the fuel structures of all countries of the world. With the increasing amount of secondary processed diesel, the trend of high sulfur degradation of diesel is also becoming more and more apparent. The sulfur oxide generated by the high-temperature combustion of sulfur-containing components in the diesel engine can not only corrode equipment and damage parts such as the engine, but also poison the tail gas treatment catalyst, reduce the catalytic activity of the tail gas treatment catalyst, increase the emission of NOx and particulate pollutants and aggravate urban environmental pollution. The production of low sulfur clean diesel oil, reducing the emission of harmful substances, has become the subject of the development of the oil refining industry today.
In the past 20 years, the requirements have not been met despite great progress in improving the combustion process of petroleum and in purifying the exhaust gas. In terms of environmental protection, there are stricter fuel quality standards in various countries. Diesel desulfurization technology is facing a great challenge due to the increasing strictness of environmental regulations, the continual upgrading of quality standards, and the increasing amount of high sulfur, poor quality diesel fuel processed. Conventional diesel hydrodesulfurization adopts a trickle bed desulfurization process, has mature technology and high reliability, but needs a large amount of hydrogen circulation to ensure the hydrogen partial pressure required by the reaction, increases the operation risk and brings huge capital investment and power consumption. To solve these problems, the U.S. ProcessDynamics company developed a liquid phase recycle hydrogenation process, i.e., the isotheramine technology, at the end of the last century. The method is characterized in that the liquid phase is a continuous phase, the gas phase is a disperse phase, the diesel oil is saturated feeding, and the hydrogen needed in the reaction is provided by dissolved hydrogen. Compared with the traditional trickle bed process, the process has the advantages that hydrogen circulation is canceled, liquid phase oil circulation is realized by adopting an interlayer hydrogen supplementing mode, concentration gradient of dissolved hydrogen is reduced, and bed temperature rise is favorably controlled. On the basis of the technology, the liquid phase circulation hydrogenation (SRH) technology and the continuous liquid phase circulation hydrogenation (SLHT) technology are developed successively. The liquid phase hydrogenation technology breaks the mass transfer limit of the traditional hydrogenation technology, effectively reduces the coking of the catalyst, but adopts a liquid phase oil circulation mode to supplement dissolved hydrogen, so that the impurity concentration is diluted, the chemical reaction driving force is reduced, the raw material residence time is reduced, and the reaction is not sufficiently efficient. Because the material contains a large amount of H2S and H2, the circulating oil pump is easy to leak, and serious consequences are caused.
The invention relates to an up-flow hydrogenation reaction device based on a tubular microporous medium foaming mechanism, which adopts microporous tube bubbling hydrogen injection to replace a large amount of circulating oil in a liquid-phase circulating hydrogenation process for hydrogen supply and multi-point hydrogen injection, so that the hydrogen is always in the states of 'dissolution and reaction at the same time' and 'micro-excessive and micro-bubbling', the concentration gradient of dissolved hydrogen in the liquid-phase oil is greatly reduced, and therefore, the coking rate of a catalyst is reduced, and the equipment cost and the coking rate of the catalyst are reduced. The key problems of the tubular microporous medium foaming continuous liquid phase hydrogenation technology are a microporous bubbling mechanism and the content of dissolved hydrogen in a microporous medium and petroleum or solvent, so that the dissolved amount of hydrogen is one of the key problems of the tubular microporous medium foaming continuous liquid phase hydrogenation technology. The process device is provided with a hydrogen chamber and a microporous tube respectively on the premise of ensuring that the liquid phase is a continuous phase, and is used for uniformly increasing the hydrogen content in the oil product so as to keep the hydrogen continuously consumed in the oil product and maintain the hydrogen partial pressure of a bed layer, accelerate the dissolution speed of the hydrogen, improve the liquid phase hydrogenation effect and be an important way for improving the continuous liquid phase hydrogenation effect.
Disclosure of Invention
Based on the purposes, the invention designs an up-flow hydrogenation reaction device based on a tubular microporous medium foaming mechanism, compared with a conventional trickle bed hydrogenation reactor, the tubular microporous medium foaming hydrogenation technology eliminates a multi-point hydrogen injection system, and instead, microporous medium continuous hydrogen injection can be used for carrying out secondary bubbling on each stage of reaction product, so that rapid dissolution of hydrogen, uniform gas-liquid distribution, high-efficiency hydrogen supplementing dispersion, reduction of 'hydrogen gradient', sufficient dissolved hydrogen and hydrogen bubbles, uniform dispersion of bubbles in raw oil, convenience in continuous liquid phase hydrogenation, capability of enhancing bubble transfer capability by timely supplementing dissolved hydrogen in a liquid phase, improvement of continuous liquid phase hydrogenation effect, reduction of N, S element content in products, and the invention is a clean production technology for low-hydrogen-consumption oil products. Meanwhile, the reaction device is combined with the gas-liquid separator, so that gas-liquid separation is realized in the device, energy consumption is saved, and separation efficiency is improved.
The technical scheme adopted by the invention is as follows:
the up-flow hydrogenation reaction device based on the tubular microporous medium foaming mechanism is characterized by comprising an outer cylinder, wherein the upper end and the lower end of the outer cylinder are respectively sealed by an upper end socket and a lower end socket, an exhaust pipe for discharging an air supply phase is arranged on the upper end socket, and a raw oil feeding pipe is arranged on the lower end socket; the inside of the outer cylinder body is provided with a plurality of tubular microporous foaming reactors through a supporting plate, the bottom of the outer cylinder body is provided with a hydrogen storage chamber and a liquid distributor, and the hydrogen storage chamber is communicated with the outside through an air inlet pipe on the side wall of the outer cylinder body to supply hydrogen and supply hydrogen into the tubular microporous foaming reactors; the liquid distributor is used for conveying the raw oil supplied by the raw oil feeding pipe into the tubular microporous foaming reactor after homogenizing and distributing the raw oil; the gas-liquid separation device comprises an outer cylinder body, an annular baffle plate, a liquid discharge pipe, a gas-liquid separation channel, a gas-liquid circulation pipeline, a liquid phase overflow flow from the upper end of the gas-liquid separation channel to an annular liquid storage chamber among the outer cylinder body, the annular baffle plate and the gas-liquid separation channel, wherein the gas-liquid separation channel is arranged above the tubular microporous foaming reactor, the bottom of the gas-liquid separation channel is connected with the annular baffle plate, the central hole of the annular baffle plate protrudes upwards to form the gas-liquid separation channel, the annular baffle plate separates the inner space of the outer cylinder body into an upper part and a lower part, raw oil flows upwards after hydrogenation reaction in the tubular microporous foaming reactor, enters the gas-liquid separation channel in the middle of the annular baffle plate, the gas phase continues to flow upwards and is discharged from the gas discharge pipe to enter the hydrogen circulation pipeline, the liquid phase overflows from the upper end of the gas-liquid separation channel to the annular liquid storage chamber between the outer cylinder body, the annular baffle plate and the gas-liquid separation channel, and the liquid discharge pipe is arranged at the bottom of the annular liquid storage chamber, and the liquid discharge pipe is used for discharging separated liquid oil out of the outer cylinder body. The upper port of the gas-liquid separation channel is also provided with an outward-expansion conical section and a direct current section which extends upwards continuously from the conical section, the conical section forms an overflow weir for increasing a gas-liquid separation surface, and the direct current section prevents liquid phase from flowing out of the separation channel at an inclined angle and then impacting the inner wall surface of the outer cylinder body.
The tubular microporous foaming reactor comprises a hydrogen chamber, microporous pipes, an oil chamber, a filler bed layer and a rotational flow guide vane, wherein the hydrogen chamber is positioned at the outermost layer, the microporous pipes are positioned in the hydrogen chamber, the upper end and the lower end of the hydrogen chamber are sealed through flange plates, the flange plates are fixed on a supporting plate to determine the distribution position of the tubular microporous foaming reactor, and the hydrogen chamber is communicated with a hydrogen storage chamber through a hydrogen distributor; the upper end and the lower end of the microporous pipe are connected with pipe bodies penetrating through the flange plates, the upper port of the pipe body at the upper end forms a liquid outlet, the lower port of the pipe body at the lower end forms a liquid inlet, the liquid inlet stretches into the liquid distributor, the device is characterized in that raw oil is introduced into the microporous tube, a plurality of groups of packing beds and oil product chambers which are distributed at intervals are arranged in the microporous tube, and a swirl making device is further arranged at the inlet position of the microporous tube.
Compared with the traditional trickle bed hydrogenation reactor, the miniature tubular microporous foaming reactor omits a multi-point hydrogen injection system, and is replaced by microporous medium hydrogen injection, the original hydrogen injection between bed layers is changed into filler bed layer coverage type hydrogen injection, hydrogen supplementing and secondary bubbling are fully carried out, the hydrogen injection quantity in each stage of reaction zone is uniform and stable, the hydrogen is fully dissolved, the hydrogen supply effect and the hydrogenation reaction efficiency are improved, meanwhile, cold hydrogen can reduce the temperature of a reaction bed layer, enhance the bubble mass transfer capability, improve the continuous liquid phase hydrogenation effect, ensure the continuity of a liquid phase while completely infiltrating a catalyst, and improve the gas-liquid two-phase mass transfer coefficient. The pore size of the microporous tube can be selected from microporous tubes of different specifications, such as 50 μm, according to the viscosity of the raw oil.
The swirl device is preferably a swirl guide vane, a plurality of blades are arranged on the guide vane, the blades are arranged in a blade groove at the bottom of the microporous tube in a welding mode, the blades of the swirl guide vane are preferably curved surfaces, the included angle between the tangent line at the top of the blades and the tangent line at the root of the blades is 60 degrees, and the swirl guide vane can be replaced by all swirl workpieces with swirl effect, such as a swirler, a spiral auger blade, a swirl groove and the like.
The upflow hydrogenation reaction device based on the tubular microporous medium foaming mechanism comprehensively considers that the working conditions of the hot high-pressure stripping separator and the microporous hydrogenation reactor are the same, combines the reaction device and the separator into reaction-separation integrated equipment, reduces the weight and the occupied area of the device, and is provided with an overflow weir to improve the separation efficiency, reduce the liquid phase outflow angle and weaken the abrasion to the inner wall surface of the reaction device. The gas-liquid separation channel is a thermal high-pressure stripping separator essentially and is used for flash evaporation to separate gas and liquid phases in a product, the gas-liquid separation channel is provided with an overflow weir, the gas-liquid separation area can be increased, the gas-liquid separation efficiency is improved, the inclined angle of the overflow weir is 45 degrees, a small direct current section is arranged at the upper part of the overflow weir, the liquid phase is prevented from flowing out of the separation channel at an inclined angle and then impacting the wall surface of the reactor, the reactor is abraded, the liquid phase flows to an annular liquid storage chamber in the reactor after being separated, and finally the liquid phase is discharged through a liquid discharge pipe arranged on an opening of the side wall of the reaction device.
By adopting the technical scheme, the invention has the following advantages and positive effects:
1. the microporous medium foaming mechanism is adopted to carry out continuous liquid-phase hydrogenation reaction, the influence of hydrogen mass transfer is avoided, vertical material flows in the reactor are liquid, the continuity of liquid phase can be ensured while the catalyst is fully infiltrated, the microporous medium is adopted to cover all filler beds for supplying hydrogen to supplement hydrogen, the hydrogen supplying effect is improved, the liquid phase on the catalyst beds in the reactor is ensured to be continuous phase, the gas phase is dispersed phase, the hydrogen is always in the states of 'side dissolution, side reaction' and 'micro excessive and micro bubbling', the rapid dissolution of the hydrogen is realized, the gas-liquid two phases are uniformly distributed, the hydrogen supplementing is efficiently dispersed, the dissolved hydrogen in the solvent can be timely supplemented, the 'hydrogen gradient' is reduced, and the reaction speed is accelerated.
2. The hydrogen needed by the hydrogenation reaction in the tubular microporous foaming reactor is provided by dissolved hydrogen, so that the reaction rate is accelerated, the gas-liquid two phases are fully contacted and dissolved for reaction, the active center of the catalyst can be more fully utilized, the total amount of the needed catalyst is reduced, the size of the reactor is reduced, the multi-point hydrogen injection can take away part of bed temperature rise, the catalyst is locally deactivated, coking is reduced, the formation and loss of light components are reduced, and the catalyst has the characteristics of low energy consumption, investment saving, small radial reaction temperature difference, less cracking products, long residence time of liquid reactants, prolonged service life of the catalyst and the like; the hydrogen required for the hydrogenation reaction is supplied by hydrogen gas dissolved in the liquid phase, and the hydrogenation reaction is controlled by the intrinsic reaction rate (catalyst efficiency and actual reaction rate), i.e., by the reaction kinetics.
3. The tubular microporous foaming reactor comprehensively considers that the upflow hydrogenation reactor and the heat Gao Fenqi extraction separator have the same working condition, and the upflow microporous foaming continuous liquid phase hydrogenation reaction separation integrated equipment is formed by combining the upflow microporous foaming reactor and the heat Gao Fenqi extraction separator, so that the total occupied area and the total mass of the device can be reduced, the operation difficulty is reduced, the heat of the product is fully reserved, and the cost is saved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an upflow hydrogenation reaction apparatus based on a tubular microporous medium foaming mechanism;
FIG. 2 is a schematic diagram of a tubular microcellular foaming reactor;
FIG. 3 is a schematic view of swirl vanes;
FIG. 4 is a schematic view of a cyclone;
FIG. 5 is a schematic diagram of an upflow microporous foaming continuous liquid phase hydrogenation process flow;
the components in the drawings are marked as follows: 1-raw oil feeding pipe, 2-liquid distributor, 3-air inlet pipe, 4-supporting plate, 5-hydrogen chamber, 6-microporous pipe, 7-oil chamber, 8-outer cylinder, 9-gas-liquid separation channel, 10-exhaust pipe, 11-liquid discharge pipe, 12-liquid outlet, 13-packed bed, 14-swirl guide vane, 15-hydrogen distributor, 16-hydrogen storage chamber, 17-liquid inlet, 18-raw oil storage tank, 19-raw oil pretreatment device, 20-oil delivery pump, 21-hydrogen oil dissolved gas tank, 22-heating furnace, 23-hydrogen storage tank, 24-thermal low-pressure separator, 25-circulating pump, 26-safety valve, 27-pressure gauge, 28-liquid level gauge and 29-dissolved gas filler.
Detailed Description
The invention is described in further detail below with reference to the embodiments of the drawings.
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described in the following specific embodiments.
Referring to the drawings, the structures, proportions, sizes, etc. shown in the drawings are shown only in connection with the disclosure of the present invention, and are not intended to limit the scope of the invention, which is defined by the claims, so that any structural modifications, proportional changes, or adjustments of sizes may be made without affecting the efficacy of the invention or achieving the purpose, and are therefore within the scope of the disclosure. In addition, the positional limitation terms recited in the present specification are used merely for convenience of description, and are not intended to limit the scope of the invention, in which the relative changes or modifications are regarded as the scope of the invention without any substantial modification to the technical content.
FIG. 1 is a schematic diagram of an upflow hydrogenation reaction device based on a tubular microporous medium foaming mechanism, and as shown in the figure, the reaction device adopts a plurality of miniature tubular microporous foaming reactors to work in parallel, so that raw oil can be uniformly dispersed, multiple pipes can be reacted step by step, the hydrogenation reaction efficiency and the product quality are improved, the generation of byproducts is reduced, and the reaction is more complete. The total process technical route of the reaction device comprises a hydrogen route, a raw oil route, a hydrogen-oil mixing reaction and a product oil-gas separation route, wherein the hydrogen route is divided into three sections, hydrogen enters a hydrogen storage chamber 16 from an air inlet pipe 3, is uniformly dispersed into a hydrogen chamber 5 of each miniature tubular microporous foaming reactor through a gas distributor 15, and is finally bubbled into an oil product chamber 7 through a microporous pipe 6, wherein the hydrogen inlet pipe 3, the hydrogen storage chamber 16 and the hydrogen chamber 5 are directly communicated, so that the uniform and stable air inlet pressure and air inflow can be ensured;
the raw oil route comprises a raw oil feeding pipe 1, a liquid distributor 2, a liquid inlet 17, a swirl guide vane 14 and an oil product chamber 7, raw oil flows from bottom to top, is uniformly dispersed by the liquid distributor 2, enters each tubular microporous foaming reactor through the liquid inlet 17, is made to rotate by the swirl guide vane 14, and shears and breaks hydrogen gas flow under high-speed rotation flow, so that the falling of bubbles is accelerated, and the gas-liquid reaction efficiency is improved; the hydrogen and the raw oil are mixed and dissolved in the oil chamber 7 of the miniature tubular microporous foaming reactor and subjected to hydrogenation reaction under the action of a catalyst to form a hydrogen-oil mixing route, after the multitube progressive hydrogenation reaction is completed, hydrogen-oil mixing reaction products flow out and gather through a liquid outlet 12 and then flow to a gas-liquid separation channel 9, namely a product oil-gas separation route, gas phases are continuously discharged upwards through an exhaust pipe 10 and can participate in hydrogen recycling, and liquid phases flow to an annular storage space in the reaction device through overflow weirs and are discharged through a liquid outlet 11, so that further separation and purification treatment can be performed, and preliminary gas-liquid separation operation is realized in the reaction device. The core technical route is a hydrogen and raw oil route, the reaction device adopts a plurality of miniature tubular microporous foaming reactors to carry out hydrogenation reaction in parallel, each tubular microporous foaming reactor is provided with a complete hydrogen and raw oil passage, unlike the traditional hydrogenation device, the tubular microporous foaming reactors utilize a microporous foaming mechanism to generate micron-sized hydrogen bubbles to strengthen the reaction, and part of hydrogen is dissolved in an oil product under the action of pressure to form hydrogen-dissolved oil, and the hydrogen-dissolved oil participates in the reaction in the form of dissolved hydrogen in the subsequent hydrogenation reaction process, so that the gas-liquid reaction is converted into liquid-liquid reaction, thereby being beneficial to continuous liquid-phase hydrogenation, improving the reaction driving force, enabling the raw materials to fully contact with a catalyst and improving the utilization rate of the catalyst.
Fig. 2 is a schematic diagram of a tubular microporous foaming reactor, as shown in the drawing, the tubular microporous foaming reactor mainly comprises a hydrogen chamber 5, a microporous tube 6, an oil chamber 7, a filler bed 13, a swirl guide vane 14, a hydrogen distributor 15, a liquid inlet 17 and a liquid outlet 12, wherein the hydrogen chamber 5 is arranged on the outer layer, the microporous tube 6 is positioned in the hydrogen chamber 5, the oil chamber 7, the filler bed 13 and the swirl guide vane 14 are all positioned in the microporous tube 6, the filler bed 13 and the oil chamber 7 comprise a plurality of groups and are all arranged above the swirl guide vane 14, the filler bed 13 and the oil chamber 7 are arranged at intervals, hydrogen in a hydrogen storage chamber 16 enters the hydrogen chamber 5 through the hydrogen distributor 15, the upper end and the lower end of the hydrogen chamber 5 are sealed by flange plates, and the flange plates are fixed on a supporting plate 4 to restrict the position of the tubular microporous foaming reactor in the whole reaction device and the relative position between each reactor. The tubular microporous foaming reactor is a main place for completing hydrogenation reaction, the reaction device adopts a plurality of tubular microporous foaming reactors to work in parallel, the number of the tubular microporous foaming reactors is more than 3, the tubular microporous foaming reactor utilizes a microporous foaming mechanism to generate micron-sized hydrogen bubbles, the pressure difference between two phases of gas and liquid is utilized, the pressure of an outer hydrogen cavity is larger than that of an inner oil cavity, high-pressure hydrogen is dispersed to form micro-air flow through microporous medium, micro bubbles are formed under the shearing and flushing action of high-speed rotating liquid and dispersed in the liquid, meanwhile, part of hydrogen is dissolved in the oil under the pressure action to form hydrogen-dissolved oil, the micro-porous medium can participate in the reaction in the form of dissolved hydrogen in the subsequent hydrogenation reaction process, the content of dissolved hydrogen can be ensured, the states of hydrogen dissolution, reaction at the same time and micro-excessive and micro-bubbling are maintained, and the microporous tube covers the whole filling bed interval, the reaction product of each stage can be directly subjected to hydrogen supplementing, and the reaction product of each stage of filling bed can be subjected to multi-time hydrogen supplementing and multi-stage micro-stage hydrogen supplementing, so that the hydrogen is uniformly distributed under the action of high-speed rotating liquid shearing flushing action, and the hydrogen supplementing effect is always in the complete hydrogen supplementing hydrogen-rich and bubbling state.
Fig. 3 and 4 are schematic diagrams of swirl vanes and swirlers, respectively. The micro-pipe type microporous foaming reactor is internally provided with a rotational flow guide vane 14, a plurality of blades are arranged on the guide vane, the blades are arranged in a blade groove at the bottom of the microporous pipe 6 through welding, the rotational flow guide vane has the function of making a rotation for a liquid phase, and the rotational flow guide vane can increase a circumferential speed for the liquid phase, so that the liquid phase can perform rotational flow movement while flowing upwards in the microporous pipe 6, the turbulent flow shearing action of the liquid phase relative to the airflow on the inner wall surface of the microporous pipe 6 is enhanced, the falling of bubbles is accelerated, the formation of air resistance is reduced, and the air inlet efficiency is further improved. The blades of the rotational flow guide vanes 14 are curved surfaces, and the included angle between the tangent line at the top of the blades and the tangent line at the root of the blades is 60 degrees; on the premise of not considering the specific air inlet efficiency improvement effect, the cyclone guide vane 14 can be replaced by all cyclone workpieces with a cyclone making effect, such as a cyclone, spiral auger blades, a cyclone groove and the like, for example, the cyclone shown in fig. 4 has the same effect as the cyclone guide vane, only the cyclone does not need to be provided with blades, a method for processing cyclone channels is adopted to guide liquid phase to do cyclone motion, the optimal number of the cyclone channels of the cyclone is 4, and the liquid phase is scattered and rotated through the cyclone channels to gather the cyclone.
The invention relates to an up-flow hydrogenation reaction device based on a tubular microporous medium foaming mechanism, which comprises the following specific working processes:
the upflow hydrogenation reaction device based on a tubular microporous medium foaming mechanism mainly comprises an upflow hydrogenation reactor outer cylinder 8 and miniature tubular microporous foaming reactors, wherein the two ends of the outer cylinder are sealed by sealing heads, an upper sealing head and a lower sealing head are respectively provided with a raw material feeding pipe 1 and a gas phase exhaust pipe 10, a plurality of miniature tubular microporous foaming reactors are arranged in the cylinder and are fixed through a supporting plate 4, the upflow hydrogenation reaction device comprises an outer hydrogen chamber 5 and an inner oil chamber 7, the two chambers are separated by tubular microporous mediums, namely a microporous pipe 6, the inner oil chamber 7 in the pipe is distributed with a multi-layer filler bed 13, swirl vanes 14, a liquid distributor 2 and a hydrogen storage chamber 16 are arranged at the bottom of the reactor, the hydrogen storage chamber 16 is connected with the hydrogen chamber 5 by the hydrogen distributor 15, the pressures of the two air chambers are equal and are controlled by the pressure of an air inlet pipe 3, the liquid distributor 2 is communicated with a liquid inlet 17, the swirl vanes 14 are arranged at the upper part of the liquid inlet 17, a gas-liquid separation channel 9 is arranged at the upper part of the liquid outlet 12, an air inlet pipe 3 of the hydrogen storage chamber 16 and a liquid outlet 11 for liquid discharging after gas-liquid separation are respectively arranged at the side wall openings of the outer cylinder, and the top of the cylinder is welded with the exhaust pipe 10.
Hydrogen enters a hydrogen storage chamber 16 through an air inlet pipe 3 with holes on the side wall of the reaction device, raw oil flows into a hydrogenation reaction device from a raw oil feed pipe 1 at the bottom of the reaction device, raw oil flows into each miniature tubular microporous foaming reactor after being uniformly dispersed by a liquid distributor 2, enters an oil chamber 7 of the reactor after being made to rotate by a cyclone guide vane 14, hydrogen enters a hydrogen chamber 5 of the reactor uniformly by a hydrogen distributor 15 under certain hydrogen pressure, hydrogen enters the oil chamber through a microporous pipe 6 of the reactor and generates a large number of tiny bubbles to perform intensified mass transfer hydrogenation reaction with the raw oil under the action of a catalyst, after multi-pipe multistage hydrogenation reaction, a product flows out from a liquid outlet and is gathered and then flows into a gas-liquid separation channel 8 to realize a preliminary gas-liquid separation process in the device, and the gas-liquid separation channel 9 is provided with an overflow weir, so that the gas-liquid separation area can be increased, the gas-liquid separation efficiency is improved, and a small section of direct current section is arranged at the upper part of the gas-liquid separation channel is prevented from flowing out of the separation channel at an inclined angle and then impacting the wall of the reactor. The separated gas phase flows out from the exhaust pipe 10 at the top of the reaction device, is recovered and treated by the subsequent process, flows into the annular liquid storage chamber in the reactor after liquid phase separation, flows out from the liquid outlet 11 on the side wall, and is subjected to the fractionation process after desulfurization and dehydrogenation.
The device is suitable for processing oil products with hydrogen not exceeding 0.6wt%, and the viscosity of the oil products is suitable for microporous medium bubbles to generate and meet the condition of rotational flow movement, so that the rotational flow shearing and crushing effects on the bubbles are facilitated. The oil product comprises straight-run diesel oil, straight-run kerosene, lubricating oil, PAO and the like. The reaction pressure of the device is 3.5-18.0 MPa, the reaction temperature is 240-400 ℃, and the hydrogen-oil volume ratio is 8-100 Nm 3 /m 3 The volume space velocity of the catalyst is 0.8 to 4.0 hours -1 . The whole hydrogenation reaction device comprises a gas-liquid two-phase temperature, pressure and flow automatic detection and adjustment control system, wherein equipment requiring the automatic detection and adjustment control system comprises a hydrogen oil dissolved gas tank and an up-flow hydrogenation reactor, and is used for maintaining stable and efficient operation of hydrogenation reaction and preventing the reactor from being blocked due to abnormal dissolved gas pressure, sintering of a packed bed and coking deactivation of a catalyst.
The invention also claims an up-flow microporous foaming continuous liquid phase hydrogenation process, as shown in fig. 5, which is a schematic diagram of an up-flow microporous foaming continuous liquid phase hydrogenation process flow, wherein the up-flow continuous liquid phase hydrogenation process flow is based on a tubular microporous medium foaming mechanism, the up-flow continuous liquid phase hydrogenation process comprises a raw material oil storage tank 18, a hydrogen oil dissolved gas tank 21, a raw material oil pretreatment device 19, a heating furnace 22 and a hydrogen storage tank 23, wherein a dissolved gas filler 29 is filled in the hydrogen oil dissolved gas tank 21, the raw material oil firstly enters the raw material oil pretreatment device 19 for pretreatment, then is pumped into the hydrogen oil dissolved gas tank 21 through an oil delivery pump 20, meanwhile, the hydrogen storage tank 23 conveys hydrogen into the hydrogen dissolved gas tank 21, part of the hydrogen in the raw material oil flows through the heating furnace 22 and then is conveyed into the up-flow hydrogenation reaction device, the solubility of the hydrogen in the oil increases along with the temperature rise, the hydrogen can be dissolved in the oil after being heated by the heating furnace, and the hydrogen content ratio of dissolved hydrogen and bubbles can be adjusted to prepare for the hydrogen in a' dissolving, a reaction while and a micro-excessive and a micro-bubbling state.
The raw oil for dissolving hydrogen enters a miniature tubular microporous foaming reactor through a raw oil feeding pipe 1, meanwhile, a hydrogen storage tank 23 continuously conveys hydrogen to an air inlet pipe 3 to provide hydrogen with pressure in a hydrogen chamber 5, after multistage hydrogenation reaction is carried out in the up-flow hydrogenation reaction device based on a tubular microporous medium foaming mechanism, the raw oil flows out from a liquid discharge pipe 11 on the side wall to a thermal low-pressure separator 24, the thermal low-pressure separator 24 is used for a gas-liquid two-phase separation process, the pressure is usually about 3MPa, after separation is completed, a gas phase enters a cold low fraction after air cooling, and a liquid phase enters a hydrogen sulfide stripping tower and then enters fractionation.
In the process flow, the side surface of the liquid distributor 2 of the up-flow hydrogenation reaction device is also provided with a circulating pipeline which is communicated with the raw oil feeding pipe 1 after passing through the circulating pump 25, so that the arrangement is that the feeding oil product has a self-circulating route before entering the microporous pipe 6, the pressure stability of the raw oil in the miniature tubular microporous foaming reactor is maintained, the self-circulation of the raw oil replaces the circulation of hydrogen supply, and the hydrogen consumption is reduced.
Preferably, the tank body of the hydrogen oil dissolved air tank 21 is also provided with a safety valve 26, a pressure gauge 27 and a liquid level gauge 28, so that an operator can observe working parameters in the hydrogen oil dissolved air tank 21 in real time, and maintenance equipment can normally operate.
While the specific embodiments of the present invention have been described above with reference to the drawings, the present invention is not limited to the protection scope of the present invention, and those skilled in the art should understand that, based on the technical solutions of the present invention, various equivalent structures or equivalent processes of the present invention may be modified or changed without any creative effort, or may be directly or indirectly applied to other related technical fields, and still fall within the protection scope of the present invention.
Claims (9)
1. The upflow hydrogenation reaction device based on the tubular microporous medium foaming mechanism is characterized by comprising an outer cylinder, wherein the upper end of the outer cylinder is provided with an exhaust pipe, and the lower end of the outer cylinder is provided with a raw oil feeding pipe; the inside of the outer cylinder body is provided with a plurality of tubular microporous foaming reactors through a supporting plate, the bottom of the outer cylinder body is provided with a hydrogen storage chamber and a liquid distributor, and the hydrogen storage chamber is communicated with the outside through an air inlet pipe on the side wall of the outer cylinder body to supply hydrogen and supply hydrogen into the tubular microporous foaming reactors; the liquid distributor is used for conveying the raw oil supplied by the raw oil feeding pipe into the tubular microporous foaming reactor after homogenizing and distributing the raw oil; a gas-liquid separation channel is arranged above the tubular microporous foaming reactor, the bottom of the gas-liquid separation channel is connected with an annular partition plate, and the central hole of the annular partition plate protrudes upwards to form the gas-liquid separation channel; a liquid discharge pipe is further arranged on the outer cylinder above the annular partition plate;
the tubular microporous foaming reactor comprises a hydrogen chamber, microporous pipes, an oil chamber, a filler bed layer and a rotational flow guide vane, wherein the hydrogen chamber is positioned at the outermost layer, the microporous pipes are positioned in the hydrogen chamber, the upper end and the lower end of the hydrogen chamber are sealed by flange plates, and the hydrogen chamber is communicated with a hydrogen storage chamber by a hydrogen distributor; the upper end and the lower end of the microporous pipe are connected with pipe bodies penetrating through the flange plates, the upper port of the pipe body at the upper end forms a liquid outlet, the lower port of the pipe body at the lower end forms a liquid inlet, and the liquid inlet extends into the liquid distributor; the microporous pipe is internally provided with a plurality of groups of packing beds and oil product chambers which are distributed at intervals, and a swirl making device is further arranged at the inlet position of the microporous pipe.
2. The upflow hydrogenation reaction apparatus according to claim 1, further characterized in that an outwardly expanding conical section and a direct current section extending upward from the conical section are further formed at the upper port of the gas-liquid separation channel, and the half cone angle of the conical section is 45 °.
3. The upflow hydrogenation reaction apparatus of claim 1, further characterized in that the swirl imparting means is a swirl vane comprising a plurality of blades, each blade being curved, the angle between the tangent at the blade tip and the tangent at the blade root being 60 °.
4. The upflow hydrogenation reaction apparatus of claim 1, further characterized in that the swirl imparting means is a cyclone, spiral auger blade, or a swirl groove structure.
5. The upflow hydrogenation reaction apparatus of claim 1, further characterized in that micropores are uniformly distributed on the microporous tube.
6. The upflow hydrogenation reaction apparatus according to claim 1, further characterized in that the upper and lower ends of the outer cylinder are respectively closed by an upper head and a lower head, the exhaust pipe is disposed on the upper head, and the raw oil feed pipe is disposed on the lower head.
7. The upflow hydrogenation reaction apparatus according to any one of claims 1 to 6, further characterized in that the operation parameters of the apparatus are set to a reaction pressure of 3.5 to 18.0MPa, a reaction temperature of 240 to 400 ℃ and a hydrogen-oil volume ratio of 8 to 100Nm 3 /m 3 The volume space velocity of the catalyst is 0.8 to 4.0 hours -1 。
8. An up-flow microporous foaming continuous liquid-phase hydrogenation process, which adopts the up-flow hydrogenation reaction device of any one of claims 1-7, and further comprises a raw oil storage tank, a hydrogen oil dissolution gas tank, a heating furnace and a hydrogen storage tank, wherein the hydrogen storage tank is internally filled with dissolved gas filler, the raw oil storage tank is communicated with a hydrogen oil dissolution gas tank pipeline after sequentially passing through a raw oil pretreatment device and an oil delivery pump, and the hydrogen oil dissolution gas tank is communicated with a raw oil feed pipe of the up-flow hydrogenation reaction device after being communicated with the heating furnace; the hydrogen storage tank is respectively communicated with the hydrogen oil dissolving tank and the air inlet pipe of the up-flow hydrogenation reaction device so as to convey hydrogen into the hydrogen oil dissolving tank and the air inlet pipe of the up-flow hydrogenation reaction device.
9. The upflow microporous foaming continuous liquid phase hydrogenation process according to claim 8, further characterized in that a circulating pipeline is further arranged on the side surface of the liquid distributor of the upflow hydrogenation reaction device, and the circulating pipeline is communicated with a raw oil feeding pipe after passing through a circulating pump.
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