CN110180471B - Slurry bed reactor and reaction system for Fischer-Tropsch synthesis - Google Patents
Slurry bed reactor and reaction system for Fischer-Tropsch synthesis Download PDFInfo
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- CN110180471B CN110180471B CN201910456696.1A CN201910456696A CN110180471B CN 110180471 B CN110180471 B CN 110180471B CN 201910456696 A CN201910456696 A CN 201910456696A CN 110180471 B CN110180471 B CN 110180471B
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- 239000002002 slurry Substances 0.000 title claims abstract description 43
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 38
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 38
- 238000011010 flushing procedure Methods 0.000 claims abstract description 92
- 239000007787 solid Substances 0.000 claims abstract description 50
- 238000012546 transfer Methods 0.000 claims abstract description 48
- 238000000926 separation method Methods 0.000 claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 29
- 239000007789 gas Substances 0.000 claims description 116
- 239000000047 product Substances 0.000 claims description 42
- 238000010992 reflux Methods 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 31
- 238000001914 filtration Methods 0.000 claims description 18
- 239000012071 phase Substances 0.000 claims description 17
- 239000007791 liquid phase Substances 0.000 claims description 13
- 238000003860 storage Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000005192 partition Methods 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 40
- 238000009826 distribution Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- 238000004062 sedimentation Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000002156 mixing Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000013461 design Methods 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 238000000429 assembly Methods 0.000 description 4
- 230000000712 assembly Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 239000002826 coolant Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- -1 aldonic ketones Chemical class 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000008258 liquid foam Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
-
- 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
- C10G2/00—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
- C10G2/30—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen
- C10G2/32—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
- C10G2/34—Apparatus, reactors
- C10G2/342—Apparatus, reactors with moving solid catalysts
- C10G2/344—Apparatus, reactors with moving solid catalysts according to the "fluidised-bed" technique
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a slurry bed reactor for Fischer-Tropsch synthesis and a reaction system, wherein the reactor comprises a reactor main body, a gas distributor arranged at the bottom of the reactor main body, a plurality of groups of heat transfer devices arranged in the reactor main body and downcomers matched with the heat transfer devices, a liquid-solid separation device is arranged between the two groups of heat transfer devices, and a gas-solid washing separation device arranged at the top of the reactor, and the reaction system comprises the reactor, a matched filtering-flushing assembly and a washing assembly. Compared with the prior art, the invention can produce Fischer-Tropsch synthesis products in an industrial scale, effectively increases the yield of target products, and reduces the catalyst loss and the difficulty of separating the catalyst from the products.
Description
Technical Field
The invention relates to a Fischer-Tropsch synthesis reactor, in particular to a slurry bed reactor for Fischer-Tropsch synthesis and a reaction system.
Background
Fischer-Tropsch synthesis (FTS for short) is a catalytic reaction that utilizes a catalyst of a group VIII metal (e.g., iron, cobalt) to convert synthesis gas (carbon monoxide and hydrogen) to Fischer-Tropsch products (primarily hydrocarbons, including aldonic ketones, etc.). Fischer-Tropsch synthesis reactors are key equipment for Fischer-Tropsch synthesis processes, and currently there are mainly two forms of fixed beds and slurry beds. The traditional fixed bed reactor has the defects of difficult temperature control, easy carbon formation of the catalyst and higher operation cost although the process is simple. The slurry bed reactor not only overcomes the defects, but also has the advantages of sufficient mixing of gas, liquid and solid phases and excellent mass and heat transfer effect, and is widely valued and applied.
The commercial use of fischer-tropsch slurry bed reactors has been a very long history, as early as the first semi-commercial demonstration of the device was built by the company Rheinpreussen germany 1953, but the device did not continue to scale up industrially due to the now international energy demand being shifted from coal to oil. The Sasol company in south Africa starts the development of the slurry bed Fischer-Tropsch reactor in the 80 th year of the 20 th century on the basis of the German slurry bed reactor, a 75-barrel/day pilot plant is built in Sasolburg in 1990, and an industrial reactor with the diameter of 5 meters and 2500 barrels/day is built in 1996, so that the Sasol company becomes the first company in the world for realizing the industrialization of the slurry bed reactor. In addition, U.S. Exoon, rentech, syntroleum has conducted research and development efforts on slurry bed Fischer-Tropsch reactors.
The core of the Fischer-Tropsch slurry bed reactor and the development of a matched system is to provide a good reaction environment and an effective product-catalyst separation method, and the related technical background is as follows:
1. Gas distributor: the experiments of R.Schafer, et al (Bubble size distributions in a bubble column reactor under industrial conditions.Experimental Thermal and Fluid Science,2002,26:595-604) show that the form of the gas distributor has great influence on the distribution of slurry beds, particularly bubbles below the penetration height, and the good gas distribution effect has important significance for preventing the bottom of a reaction zone from being excessively mild and the distributor from being blocked. Patent CN1283349C discloses a slurry bed reactor employing a nozzle and a secondary distribution plate, the nozzle outlet has a spherical device for preventing slurry backflow, so as to solve the problems of blockage of the distributor and uneven gas distribution. The main problems are that the distributor is complex in structure and difficult to maintain, and the nozzles are easy to be blocked when the system is stopped.
2. False bottom: patent CN1233454C discloses a false bottom design with riser, the distance between the false bottom and the gas distributor is small, the catalyst is not easy to deposit at the bottom of the reactor, and the problem of local overheating caused by the false bottom is avoided. The main problem is that the opening of the false bottom affects the mechanical strength of the false bottom.
3. Heat transfer device: marretto and Krishna(Design and optimization of a multi-stage bubble column slurry reactor for Fischer-Tropsch.Catalysis Today,2001,66:241-248) propose a tubular heat exchanger for a fischer-tropsch slurry bed reactor consisting of two plenums and a tube bundle of tubes connected thereto, boiler feed water flowing down the center of the tubes and back up the peripheral annular zone. Patent CN100522335C discloses a cooling tube apparatus for a fischer-tropsch synthesis reactor, the cooler being composed of a plurality of tube bundle assemblies and lumped tubes connected thereto, each tube bundle assembly being composed of 4 or 6 tubes and two plenums connected thereto, the design being capable of simplifying the removal and reinstallation of the cooling tubes. Due to the structural characteristics of the cooler, the heat exchange tubes in the reactor are low in arrangement density, and the heat exchange capacity of the cooler is limited under the conditions of high catalyst concentration or emergency.
4. And a down-comer. Patent US6201031 discloses a slurry bed reactor with a downcomer, and proposes the working principle of the downcomer and the calculation method of the slurry conveying quantity. The industrial test results disclosed in patent US5382748 show that the downcomer has a significant improvement in the axial concentration distribution and temperature distribution of the catalyst. However, the above patent does not mention critical issues of downcomer size, placement, design principles, etc.
5. Liquid-solid separation device and filtration flushing subassembly. Patent CN1233453C discloses an automatic filtration/flushing device for liquid-solid separation of slurry bed reactor, which adopts a tube array structure and implements periodic filtration/flushing through a program-controlled valve installed on the main pipe.
6. Gas-solid washing separation device and washing subassembly. Patent US6265452 discloses a scheme for arranging a plurality of trays at the top of the reactor, above which reflux condensate is introduced to scrub the gas product, in order to reduce the catalyst content in the gas. The tower tray used in the design scheme is similar to the tower tray of the rectifying tower, is very easy to be blocked by the catalyst, and further influences the washing effect and the safety of the device.
As is known in the art, the fischer-tropsch reaction is very sensitive to temperature and gas-liquid-solid three-phase flow mixing, and the difficulty of product-catalyst separation is great. Optimizing the reactor design and product separation scheme can effectively improve the efficiency and stability of the Fischer-Tropsch slurry bed reactor. The prior art generally has the problems of poor mass and heat transfer effect in the reactor, complex product-catalyst separation method and the like.
Chinese patent CN1233451C discloses a gas-liquid-solid three-phase slurry-state industrial reactor capable of continuous operation, which comprises an inlet gas distribution component for uniformly distributing gas, one or more layers of heat exchange tube components for heating/cooling the bed, one or more layers of liquid-solid separator components capable of automatic cleaning, and an outlet dedusting and demister component for removing liquid foam and solid entrainment. However, the patent does not provide a depressurization tube, and therefore, the generation of dead zones and hot spots at the bottom of the bed cannot be avoided.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a slurry bed reactor and a reaction system which are suitable for the Fischer-Tropsch synthesis technology and are used for continuously producing Fischer-Tropsch synthesis products. Fischer-Tropsch products refer to hydrocarbons (carbon numbers in the range of 1 to 70 and even higher) and oxygenates (aldonic ketones), which are classified into liquid Fischer-Tropsch wax and gaseous hydrocarbon products, depending on the phase at the operating conditions.
The aim of the invention can be achieved by the following technical scheme:
A slurry bed reactor for fischer-tropsch synthesis comprising
The main body of the reactor is provided with a plurality of grooves,
A gas distributor arranged at the bottom of the reactor main body,
A plurality of groups of heat transfer devices arranged in the reactor main body and a downcomer matched with the heat transfer devices, a liquid-solid separation device is arranged between the two groups of heat transfer devices,
And the gas-solid washing and separating device is arranged at the top of the reactor.
The raw material gas is introduced into the reactor and mixed with Fischer-Tropsch wax and catalyst filled in the reactor, wherein the raw material gas refers to synthesis gas (carbon monoxide and hydrogen) produced by a gas production unit (such as coal gas, natural gas conversion and the like) or mixed gas of the synthesis gas and other process gases (such as non-condensable gas in gas products and the like). Under certain temperature and pressure conditions, carbon monoxide and hydrogen are converted into Fischer-Tropsch products on the surface of the catalyst and a large amount of heat is released. Specifically, the Fischer-Tropsch synthesis catalyst is one or a mixture of iron, cobalt and other VIII metal catalysts, and the average particle size is 40-150 mu m. The operating pressure is 1.0-5.0 MPaG, the operating temperature is 200-300 ℃, and the apparent gas velocity is 0.2-0.5 m/s.
The reactor main body is a vertical pressure vessel, and the diameter of the reactor is designed according to the inlet synthetic gas flow and apparent gas velocity, and is generally 0.5-15 m; the tangential height of the reactor comprises the height of the reaction zone, the size and the installation height of internal components such as a gas-solid washing and separating device, a false bottom and the like, and is generally 30-60 m.
A false bottom is arranged between the bottom end enclosure connected with the bottom of the reactor main body and the gas distributor, the false bottom is a round partition plate, a false bottom area isolated from the reaction area is formed by the false bottom and the bottom end enclosure, and a balance pipe is arranged between the false bottom area and the outlet of the reactor. The radian of the baffle plate is as small as possible, so that the effect of optimizing the gas distribution at the bottom of the reaction zone is achieved. The false bottom is flushed by the gas sprayed by the gas distributor, so that the dead bed area caused by too large radian of the bottom seal head (generally conical or ellipsoidal) can be effectively avoided. The distance between the false bottom and the nozzle outlet is 0.1-0.5 m, and the flushing speed is 30-80 m/s.
In order to ensure that the deformation of the false bottom and the sealing structure (such as a welding seam) at the joint of the false bottom and the shell is within an allowable range, a balance pipeline is arranged below the false bottom besides a supporting piece so that the pressure at two sides of the false bottom is in a balanced state. The support member can be one or a combination of two of a cross beam and a support post, and is fixed on the reactor cylinder or the bottom sealing head to support the vertical downward stress of the false bottom. The balance pipeline is connected with the inlet gas of the reactor generally, so that the pressure of the gas above and below the false bottom is kept the same, and the excessive deformation of the false bottom caused by the excessive pressure difference at the two sides of the false bottom is prevented.
The gas distributor can be a concentric circular or branch-shaped multi-pipe distributor, the main pipe is radially extended to the wall surface by taking the feeding pipe as the center of a circle, and the branch pipes uniformly cover the radial plane. The lower part of the distribution pipe is provided with nozzles which are vertically downward, and the distances between adjacent nozzles are similar or equal. Specifically, the aperture of the nozzle is 5-25 mm, the pressure drop is 0.02-0.1 MPa, and the linear velocity of the outlet is 50-100 m/s. In order to prevent slurry from flowing back into the gas distributor and catalyst from depositing at the bottom under the stop state, an emergency nitrogen pipeline connected with the feeding pipeline or the gas distributor is configured, and the emergency nitrogen pipeline is immediately led into the reactor when the feeding synthesis gas is interrupted, so that the apparent gas velocity in the reactor is kept to be not lower than the settling velocity of the catalyst particles with the maximum particle size, and is generally not lower than 0.1m/s. .
The heat transfer device consists of an inlet collecting pipe, an outlet collecting pipe and a plurality of groups of heat transfer coils which are connected in parallel, and 2-3 layers are arranged along the axial direction of the reactor. A heat transfer device comprises 2-4 pairs of inlet and outlet collecting pipes, wherein the form of the collecting pipes can be an arc pipe close to the wall surface of a reactor or a straight pipe penetrating into the center of the reactor in the radial direction. The heat transfer coil consists of 2-60 straight pipes connected in series through 180 deg elbow, and the inlet and outlet are connected to the inlet and outlet lumped pipes. The straight pipe form can also adopt special-shaped pipes such as corrugated pipes, finned pipes and the like besides the light pipe to enhance the wall surface heat exchange of the slurry side, and the length is 6-10 m. The number of straight pipes of each group of heat transfer coils is equal to ensure that the water flow of each group of boilers is uniformly distributed. If the tube side pressure drop of the collecting and collecting tube is larger than the pressure drop of a single cooling tube, the number of the cooling tubes of the heat transfer coil connected with the far end of the collecting and collecting tube is reduced. The temperature of the boiler water supply at the inlet of the heat transfer device is 20-80 ℃ lower than the temperature of the reaction zone in the reactor, the reaction heat is absorbed through convection-wall surface heat exchange, partial reaction is converted into saturated steam, and the gasification rate at the outlet is 0.05-0.25.
The downcomer is a special inner member for enhancing the gas-liquid-solid three-phase mixing, and the working principle is as follows: the gas-liquid-solid three-phase flow enters a sedimentation pipe with larger diameter in a bypass way, large bubbles continue to move upwards under the action of buoyancy, and the slurry is settled in the pipe under the action of gravity, so that a region with low gas content and high density is formed in the sedimentation pipe; the slurry with the large bubbles removed moves downwards under the action of gravity and flows to the area below the bed layer through the conveying pipe. The downward slurry flow in the down-flow pipe and the upward three-phase flow in the reaction zone form a fluid circulation loop, and the stirring effect is achieved. Generally, the diameter of the sedimentation tube of the downcomer is 0.2-1.5 m, the diameter of the delivery tube is 0.1-0.7 m, and the area of each layer of sedimentation tube accounts for 10-30% of the sectional area of the reaction zone.
In order to enhance the mixing of the slurry around the cooler and improve the convective heat transfer efficiency of the slurry side, the downcomer is used in combination with the heat transfer device to form a stirring zone around the heat transfer device. Because of the high center and low near wall of the bubble diameter and velocity in the reaction zone under the shearing force of the wall facing the three-phase flow, the downcomers should be uniformly arranged at the center and near wall positions of the reactor in order to make the radial distribution of the three-phase flow more uniform. Specifically, the downcomers are arranged in the axle center or symmetrically around the axle center, and the center distance between adjacent downcomers is 0.5-2 m.
The liquid-solid separation device is composed of 5-30 groups of filter components, and each group of filter components is composed of 5-30 filter elements, a filter collecting main pipe and a flushing collecting main pipe which are connected with the filter elements. The form of the filter element can be selected from sintered metal, porous ceramic and the like, the maximum particle size of the catalyst allowed to pass through is 10-40 mu m, and the catalyst content in the filtered slurry is less than 100ppm. The filtered fischer-tropsch wax entrains a significant amount of gaseous product and synthesis gas and in order to prevent air lock, filtrate is led out of the filter element from above into the filter header and correspondingly below into the flushing header.
When the cooler is arranged in two layers, the liquid-solid separation device is arranged between the two layers of heat transfer devices; when the heat transfer device is three-layered, the liquid-solid separation device is preferably installed between the top and middle heat transfer devices to reduce the carbon monoxide and hydrogen content of the entrained gas. In order to ensure that the filtration and flushing volumes of each set of filter assemblies are equal, the number of filter elements should be as equal as possible.
The gas-solid washing and separating device consists of a backflow wax sprayer, a backflow condensate sprayer, a liquid distributor and a gas-liquid separator; the reflux wax sprayer is arranged below the reflux condensate sprayer, the liquid distributor is arranged below the reflux condensate sprayer, and the gas-liquid separator is arranged above the reflux condensate sprayer and the liquid distributor and is connected with a gas outlet at the top of the reactor.
The gas-solid washing and separating device washes a gas product by using a medium with lower catalyst content, and then removes tiny liquid drops containing solid particles in the gas product so as to achieve the effect of reducing the catalyst content in the gas product, wherein the device comprises a sprayer for uniformly distributing chilling liquid, a liquid distributor for strengthening gas-liquid contact and a gas-liquid separator for separating liquid drops/product gas. The gaseous product leaving the reaction zone is countercurrently contacted with Fischer-Tropsch wax having a relatively low catalyst content (< 100 ppm) on a liquid distributor below the return wax spray, and the majority of entrained catalyst-containing entrainment is absorbed by the return wax and carried back to the reaction zone. The gas product is then contacted in countercurrent with reflux condensate which is almost free of catalyst (< 5 ppm), the catalyst being further replenished. In addition, the condensing action of the reflux condensate on the gas product causes gas-liquid two-phase mass transfer, so that the washing effect can be further enhanced. The chilled gas product and the entrainment which is carried by the chilled gas product and almost does not contain the catalyst enter a gas-liquid separator, the entrainment collides with and is attached to a baffle plate, then the entrainment flows back to a liquid distributor along the baffle plate, and the gas product flows out of the reactor through the baffle plate.
The reaction system provided by the invention comprises a reactor, and a filtering-flushing assembly and a washing assembly which are connected with the reactor.
The filter-flushing assembly consists of a Fischer-Tropsch wax collecting tank, a Fischer-Tropsch wax buffer tank, a filter, a flushing wax collecting tank, a flushing pump, a flushing wax tank, a filter valve and a flushing valve, wherein an inlet of the Fischer-Tropsch wax collecting tank is connected with a filtering lumped pipe of the liquid-solid separation device through a pipeline provided with the filter valve, a liquid phase outlet is connected with the Fischer-Tropsch wax buffer tank, a liquid phase outlet of the Fischer-Tropsch wax buffer tank is connected with the filter, a filtrate outlet of the filter is connected with the flushing wax collecting tank, a liquid phase outlet of the flushing wax collecting tank is connected with the flushing pump, an outlet of the flushing pump is connected with the flushing wax tank, and a liquid phase outlet of the flushing wax tank is connected with the flushing lumped pipe of the liquid-solid separation device through a pipeline provided with the flushing valve.
The flushing assembly can also be a gas flushing assembly, the flushing wax collecting tank and the flushing wax tank are high-pressure gas storage tanks, and flushing gas in the high-pressure gas storage tanks is synthetic gas or inert gas.
The purpose of the filter-flushing assembly is to filter the Fischer-Tropsch wax and flush the liquid-solid separation device within the reactor. The filtration-flushing operation procedure includes filtration, flushing and optionally waiting conditions, by controlling the filter valve and the flushing valve associated with the liquid-solid separation device. Specifically, when one or more groups of filter components are switched from a filtering state to a flushing state, one scheme is that the same number of groups of filter components are switched to a waiting state, and the filter components are switched to the filtering state after the waiting state is finished, and the steps are repeated in sequence; another proposal is that the filter state is directly switched to the flushing state after the end, and the filter state is repeatedly performed in turn. In the filtering state, the filter valve is opened, the flushing valve is closed, and the duration time is 10-30 min; in the waiting state, the filter valve is closed, the flushing valve is closed, and the duration time is 5-20 min; in the flushing state, the filter valve is closed, and the flushing valve is opened for 2-20 s.
The fine filtration of the Fischer-Tropsch wax is achieved by the following scheme: the Fischer-Tropsch wax separated by the liquid-solid separation device enters a Fischer-Tropsch wax collecting tank to remove entrained gas products and synthesis gas. The degassed Fischer-Tropsch wax enters a Fischer-Tropsch wax buffer tank for decompression and then enters a filter. The filter type can be selected from vane type or plate frame type. After fine filtration, the maximum particle size of the catalyst in the Fischer-Tropsch wax is less than 1 mu m, and the content is less than 5ppm. Part of the Fischer-Tropsch wax after fine filtration is extracted as a product, and the other part is led into a flushing wax collecting tank. The flushing wax is conveyed to a flushing wax tank through a flushing pump and then returned to the reactor for flushing the liquid-solid separation device. Wherein the pressure of the Fischer-Tropsch wax collecting tank is lower than 0.1-1.0 MPa of the reactor, the pressure of the Fischer-Tropsch wax buffering tank is lower than the allowable pressure of the filter, and the pressure of the wax flushing tank is higher than 0.1-1.0 MPa of the reactor.
The washing assembly consists of a product gas cooler, a condensate separating tank, a condensate reflux pump and a Fischer-Tropsch wax reflux pump, wherein an inlet of the product gas cooler is connected with a gas outlet of the reactor, an outlet of the product gas cooler is connected with the condensate separating tank, an oil phase outlet of the condensate separating tank is connected with the condensate reflux pump, an outlet of the condensate reflux pump is connected with a condensate sprayer of the gas-solid washing and separating device, an inlet of the Fischer-Tropsch wax reflux pump is connected with the Fischer-Tropsch wax collecting tank, and an outlet of the Fischer-Tropsch wax reflux pump is connected with the reflux wax sprayer.
And the washing component condenses and separates the gas product, and conveys the oil phase condensate and the Fischer-Tropsch wax separated by the liquid-solid separation device to the washing and separation device. The gas at the outlet of the reactor enters a cooler and is cooled to 20-150 ℃, and water and heavy hydrocarbon in the gas are condensed into liquid. The cooler may employ one or a combination of more of the following coolers depending on the process requirements: precooler using inlet synthesis gas or other process fluid with lower temperature as cooling medium; a water cooler using circulating water as a cooling medium; an air cooler using air as a cooling medium. And the cooled gas enters a condensate separating tank to carry out gas-oil-water three-phase separation. And taking a part of the oil phase condensate as a product, and conveying a part of the oil phase condensate to a condensate sprayer through a condensate reflux pump. The return wax pump delivers the Fischer-Tropsch wax in the Fischer-Tropsch wax collecting tank to the return wax shower. Wherein the liquid-gas ratio of condensate to gas product is 2-4L/m 3, the liquid-gas ratio of reflux wax to gas product is 0.4-1L/m 3, and the temperature of gas product after chilling is lower than the temperature of reaction zone by 10-60 ℃.
Compared with the prior art, the invention has the following advantages:
(1) The inlet gas distributor is matched with the false bottom to effectively improve the gas-liquid-solid mixing at the bottom of the reaction zone, and avoid the occurrence of a dead bed zone at the bottom. The pressure difference at two sides of the false bottom can be fluctuated in a small range even under extreme conditions by the pressurizing and balancing pipeline, so that the safety of the false bottom and the sealing element thereof is ensured.
(2) The heat transfer device has simple structure and large pipe distribution density, can ensure sufficient heat exchange area, and is suitable for various complex working conditions and larger load change.
(3) The reasonable size and arrangement mode of the downcomers can obviously improve the three-phase mixing of gas, liquid and solid, and the heat exchange effect can be enhanced when the downcomers are matched with a heat transfer device.
(4) The liquid-solid separation device and the filtering-flushing assembly are simple and efficient to operate, and the catalyst content of the Fischer-Tropsch wax can be effectively reduced, so that the catalyst can meet the requirements of flushing and product quality.
(5) The gas-solid washing and separating device and the washing component can effectively remove the catalyst in the gas product, reduce the loss of the catalyst and reduce the risk of blocking downstream equipment.
(6) Compared with the technical scheme disclosed by CN1233451C, the three-phase mixing in the bed is enhanced by configuring the downcomer, more reasonable distributor configuration is adopted, the generation of dead zones and hot spots at the bottom of the bed is restrained, the temperature difference in the bed is further reduced, and the yield of target products is improved.
Drawings
FIG. 1 is a schematic structural view of a reactor;
FIG. 2 is a schematic view of the structure of a filter-rinse assembly associated with the reactor;
FIG. 3 is a schematic view of the structure of a washing assembly matched with the reactor.
In the figure, 1 is a reactor main body, 2 is a gas distributor, 3 is a false bottom, 4 is a heat transfer device, 4a is a heat transfer coil, 4b is an inlet header, 4C is an outlet header, 5 is a downcomer, 5a is a sedimentation pipe, 5b is a conveying pipe, 6 is a liquid-solid separation device, 6a is a filtering header, 6b is a flushing header, 6C is a filter element, 7 is a gas-solid washing separation device, 7a is a backflow wax sprayer, 7b is a backflow condensate sprayer, 7C is a liquid distributor, 7d is a gas-liquid separator, 8 is a reaction zone, 9 is a false bottom zone, S1 is a raw material gas, S2 is a gas product, S3 is boiler feed water, S4 is byproduct steam, S5 is produced Fischer-Tropsch wax, S6 is flushing wax, S7 is backflow wax, S8 is backflow condensate, S9 is a pressurizing pipe, S10 is a balance pipe, S11 is backflow Fischer-Tropsch wax, V1 is a Fischer-Tropsch wax collecting tank, V2 is a slow wax tank, V3 is a backflow wax tank, V1 is a backflow condensate liquid condensate sprayer, V1 is a flushing pump, V1 is a flushing valve, P1 is a flushing tank, and P1 is a flushing valve.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
In the description of the present invention, it should be understood that the terms "above," "bottom," "parallel," "intermediate," and the like indicate an orientation or a positional relationship, and are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the components or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Example 1
The slurry bed reactor for Fischer-Tropsch synthesis structurally comprises a reactor main body 1, a gas distributor 2 arranged at the bottom of the reactor main body 1, a plurality of groups of heat transfer devices 4 arranged in the reactor main body 1 and downcomers 5 matched with the heat transfer devices 4, a liquid-solid separation device 6 is arranged between the two groups of heat transfer devices 4, and a gas-solid washing separation device 7 is arranged at the top of the reactor main body 1.
The reactor main body 1 is a vertical pressure vessel, a false bottom 3 is arranged between a bottom sealing head connected with the bottom of the reactor main body 1 and the gas distributor 2, the false bottom 3 is a circular partition plate, a false bottom region 9 isolated from the reaction region is formed by the false bottom 3 and the bottom sealing head, and a pressurizing pipe S9 and a balancing pipe S10 are arranged between the false bottom region 9 and the reactor outlet.
The gas distributor 2 is a multitube distributor and is connected with a raw gas inlet, and a gas outlet is vertically downward. The heat transfer device 4 consists of an inlet collecting main 4b, an outlet collecting main 4c and a plurality of groups of heat transfer coils 4a which are connected in parallel, wherein the inlet and the outlet of the heat transfer coils 4a are respectively connected with the inlet collecting main 4b and the outlet collecting main 4 c. The downcomer 5 consists of a funnel-shaped sedimentation tube 5a and a conveying tube 5b connected with the bottom of the sedimentation tube 5a, the top end of the sedimentation tube 5a is arranged above the heat transfer device 4, the conveying tube 5b is parallel to the heat transfer coil 4a, and the bottom end of the sedimentation tube 5a is arranged below the heat transfer device 4.
The liquid-solid separation device 6 is composed of a plurality of groups of filter components, each group of filter components is composed of a plurality of filter elements 6c and two lumped tubes, the lower ends of the filter elements 6c are connected with the filter collecting main 6a, and the upper ends of the filter elements are connected with the flushing collecting main 6b. The gas-solid washing and separating device 7 consists of a backflow wax sprayer 7a, a backflow condensate sprayer 7b, a liquid distributor 7c and a gas-liquid separator 7 d; the reflux wax sprayer 7a is arranged below the reflux condensate sprayer 7b, the liquid distributor 7c is arranged below the reflux condensate sprayer, and the gas-liquid separator 7d is arranged above the reflux condensate sprayer 7b and the liquid distributor 7c and is connected with a gas outlet at the top of the reactor.
Feed gas S1 enters the reactor body 1 from the false bottom zone 9. In the reaction zone 8, the final gas product S2 is extracted from the top of the reactor body 1, boiler feed water S3 enters the heat transfer device 4 through the inlet collecting main 4b, and byproduct steam S4 obtained through heat exchange is discharged from the outlet collecting main 4 c. In the reaction zone 8, the flushing wax S6 enters the liquid-solid separation device 6 through a flushing header pipe 6b, and the extracted fischer-tropsch wax S5 is extracted through a filtering header pipe 6 a. In the gas-solid washing and separating device 7, the return wax S7 enters from the return wax sprayer 7a, and the return condensate S8 enters from the return condensate sprayer 7 b.
A slurry bed reaction system for fischer-tropsch synthesis comprising a reactor, and a filter-rinse assembly and a wash assembly connected to the reactor.
The structure of the filtering-flushing assembly is shown in fig. 2, and the filtering-flushing assembly consists of a Fischer-Tropsch wax collecting tank V1, a Fischer-Tropsch wax buffering tank V2, a flushing wax collecting tank V3, a flushing wax tank V4, a fine filter F1, a matched filtering valve VLV1, a flushing valve VLV2, a flushing wax pump P1 and other assemblies. The inlet of the Fischer-Tropsch wax collecting tank V1 is connected with a filtering collecting main pipe 6a provided with a filtering valve VLV1 and a liquid-solid separating device 6, receives the extracted Fischer-Tropsch wax S5, and can also extract the reflux Fischer-Tropsch wax S11. The liquid phase outlet of the Fischer-Tropsch wax collecting tank V1 is connected with the Fischer-Tropsch wax buffer tank V2, the liquid phase outlet of the Fischer-Tropsch wax buffer tank V2 is connected with the fine filter F1, the filtrate outlet of the fine filter F1 is connected with the flushing wax collecting tank V3, the liquid phase outlet of the flushing wax collecting tank V3 is connected with the flushing pump P1, the outlet of the flushing pump P1 is connected with the flushing wax tank V4, and the liquid phase outlet of the flushing wax tank V4 is connected with the flushing collecting pipe 6b of the liquid-solid separation device 6 by a pipeline provided with a flushing valve VLV 2.
The structure of the washing assembly is shown in fig. 3, and the washing assembly is composed of a product gas cooler C1, a condensate separating tank V5, a condensate reflux pump P3, a Fischer-Tropsch wax reflux pump P2 and other assemblies. The inlet of the product gas cooler C1 is connected with the gas outlet of the reactor, the gas product S2 is led in, the outlet is connected with the condensate separating tank V5, the oil phase outlet of the condensate separating tank V5 is connected with the condensate reflux pump P3, the outlet of the condensate reflux pump P3 is connected with the reflux condensate sprayer 7b of the gas-solid washing and separating device 7, the inlet of the Fischer-Tropsch wax reflux pump P2 is connected with the Fischer-Tropsch wax collecting tank V1, the Fischer-Tropsch wax S11 is received, the outlet is connected with the reflux wax sprayer 7a, and the reflux wax S7 is output.
Example 2
The slurry bed reaction system for Fischer-Tropsch synthesis is substantially the same as that of example 1, except that in this example the flushing assembly is a gas flushing assembly, the flushing wax collecting tank and the flushing wax tank used are both high pressure gas storage tanks, and the flushing gas in the high pressure gas storage tanks is synthesis gas or inert gas.
Example 3
The technical solution in this example comprises a slurry bed reactor as shown in fig. 1, a filter-rinse assembly as shown in fig. 2 and a wash assembly as shown in fig. 3. The reactor tangential height was 45m and the internal diameter was 0.52m. The reaction zone 8 was charged with Fischer-Tropsch precipitated iron catalyst, and the feed synthesis gas S1 gas flow was 320000Nm 3/h, where the hydrogen to carbon ratio in the synthesis gas from the gas unit was 2:1. Reaction zone 8 was operated at a pressure of 2.3MPaG and at a temperature of 240 ℃. The yield of the Fischer-Tropsch wax is 4.8t/h, the catalyst content in the produced Fischer-Tropsch wax S5 is 80ppm, and the catalyst content in the filtered Fischer-Tropsch wax is less than 5ppm by a filter F1. The gas product condensate was 7.0t/h, with a catalyst content of <5ppm.
Example 4
The reactor and associated system described in example 1 were used. The reaction zone 8 was charged with Fei Tuogu-based catalyst and the amount of fed synthesis gas S1 was 328000Nm 3/h, where the hydrogen to carbon ratio in the synthesis gas from the gas unit was 2:1. Reaction zone 8 was operated at a pressure of 2.3MPaG and at a temperature of 240 ℃. The yield of the Fischer-Tropsch wax is 4.8t/h, the catalyst content in the produced Fischer-Tropsch wax S5 is 80ppm, and the catalyst content in the filtered Fischer-Tropsch wax is less than 5ppm by a filter F1. The gas product condensate was 6.7t/h, with a catalyst content of <5ppm.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (8)
1. A slurry bed reactor for Fischer-Tropsch synthesis, comprising
The main body of the reactor is provided with a plurality of grooves,
A gas distributor arranged at the bottom of the reactor main body,
A plurality of groups of heat transfer devices arranged in the reactor main body and a downcomer matched with the heat transfer devices, a liquid-solid separation device is arranged between the two groups of heat transfer devices,
The gas-solid washing and separating device is arranged at the top of the reactor;
the reactor main body is a vertical pressure vessel, a false bottom is arranged between a bottom head connected with the bottom of the reactor main body and the gas distributor, the false bottom is a circular partition plate, a false bottom area isolated from the reaction area is formed by the false bottom and the bottom head, and a balance pipe is arranged between the false bottom area and the reactor outlet;
the gas-solid washing and separating device consists of a backflow wax sprayer, a backflow condensate sprayer and a liquid distributor and liquid separator; the reflux wax sprayer is arranged below the reflux condensate sprayer, the liquid distributor is arranged below the reflux condensate sprayer, and the gas-liquid separator is arranged above the reflux condensate sprayer and the liquid distributor and is connected with a gas outlet at the top of the reactor.
2. A slurry bed reactor for fischer-tropsch synthesis according to claim 1, wherein the gas distributor is a multitube distributor connected to the feed gas inlet and the gas outlet is directed vertically downwards.
3. A slurry bed reactor for fischer-tropsch synthesis according to claim 1, wherein the heat transfer device comprises an inlet header pipe, an outlet header pipe and a plurality of groups of heat transfer coils connected in parallel, and the inlet and outlet of the heat transfer coils are respectively connected with the inlet header pipe and the outlet header pipe.
4. A slurry bed reactor for fischer-tropsch synthesis according to claim 1, wherein the downcomer comprises a funnel-shaped settling tube and a transfer tube connected to the bottom thereof, the top end of the settling tube being above a heat transfer device, the transfer tube being parallel to the heat transfer coil, the bottom end of the settling tube being arranged below the heat transfer device.
5. A slurry bed reactor for fischer-tropsch synthesis according to claim 1, wherein the liquid-solid separation device comprises a plurality of groups of filter elements, each group of filter elements comprising a plurality of filter elements and two lumped tubes, the lower ends of the filter elements being connected to a filter header pipe and the upper ends being connected to a flushing header pipe.
6. A slurry bed reaction system for fischer-tropsch synthesis comprising a reactor according to any one of claims 1 to 5 and a filter-rinse assembly and a wash assembly connected to the reactor.
7. A slurry bed reaction system for Fischer-Tropsch synthesis according to claim 6, wherein,
The filter-flushing assembly consists of a Fischer-Tropsch wax collecting tank, a Fischer-Tropsch wax buffer tank, a filter, a flushing wax collecting tank, a flushing pump, a flushing wax tank, a filter valve and a flushing valve, wherein an inlet of the Fischer-Tropsch wax collecting tank is connected with a filtering lumped pipe of the liquid-solid separation device through a pipeline provided with the filter valve, a liquid phase outlet is connected with the Fischer-Tropsch wax buffer tank, a liquid phase outlet of the Fischer-Tropsch wax buffer tank is connected with the filter, a filtrate outlet of the filter is connected with the flushing wax collecting tank, a liquid phase outlet of the flushing wax collecting tank is connected with the flushing pump, an outlet of the flushing pump is connected with the flushing wax tank, and a liquid phase outlet of the flushing wax tank is connected with the flushing lumped pipe of the liquid-solid separation device through a pipeline provided with the flushing valve;
The washing assembly consists of a product gas cooler, a condensate separating tank, a condensate reflux pump and a Fischer-Tropsch wax reflux pump, wherein an inlet of the product gas cooler is connected with a gas outlet of the reactor, an outlet of the product gas cooler is connected with the condensate separating tank, an oil phase outlet of the condensate separating tank is connected with the condensate reflux pump, an outlet of the condensate reflux pump is connected with a condensate sprayer of the gas-solid washing and separating device, an inlet of the Fischer-Tropsch wax reflux pump is connected with the Fischer-Tropsch wax collecting tank, and an outlet of the Fischer-Tropsch wax reflux pump is connected with the reflux wax sprayer.
8. A slurry bed reaction system for fischer-tropsch synthesis according to claim 7, wherein the flushing assembly is a gas flushing assembly, the flushing wax collecting tank and the flushing wax tank are high pressure gas storage tanks, and the flushing gas in the high pressure gas storage tanks is synthesis gas or inert gas.
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