WO2014121718A1 - Slurry-bed reaction equipment and usage thereof - Google Patents

Slurry-bed reaction equipment and usage thereof Download PDF

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Publication number
WO2014121718A1
WO2014121718A1 PCT/CN2014/071647 CN2014071647W WO2014121718A1 WO 2014121718 A1 WO2014121718 A1 WO 2014121718A1 CN 2014071647 W CN2014071647 W CN 2014071647W WO 2014121718 A1 WO2014121718 A1 WO 2014121718A1
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WO
WIPO (PCT)
Prior art keywords
slurry
section
gas
reaction
separator
Prior art date
Application number
PCT/CN2014/071647
Other languages
French (fr)
Inventor
Simon Xiaomang ZHANG
Yanning LUO
Zhengxing JIANG
Jiangfeng WANG
Qinghua BAO
Yan Chen
Liang Huang
Jinping LI
Yaning XIAO
Dongfei WANG
Yuhan Sun
Xiaohao LIU
Bo LIAO
Angelo AMORELLI
Original Assignee
Shanghai Bi Ke Clean Energy Technology Co., Ltd.
Shanxi Lu'an Environmental Energy Development Co. Ltd.
Shanghai Advanced Research Institute, Chinese Academy Of Sciences
Bp (China) Holdings Limited
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Filing date
Publication date
Application filed by Shanghai Bi Ke Clean Energy Technology Co., Ltd., Shanxi Lu'an Environmental Energy Development Co. Ltd., Shanghai Advanced Research Institute, Chinese Academy Of Sciences, Bp (China) Holdings Limited filed Critical Shanghai Bi Ke Clean Energy Technology Co., Ltd.
Publication of WO2014121718A1 publication Critical patent/WO2014121718A1/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20Chemical 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
    • B01J8/22Chemical 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005Separating solid material from the gas/liquid stream
    • B01J8/0055Separating solid material from the gas/liquid stream using cyclones
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2/00Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
    • C10G2/30Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen
    • C10G2/32Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
    • C10G2/34Apparatus, reactors
    • C10G2/342Apparatus, reactors with moving solid catalysts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00477Controlling the temperature by thermal insulation means
    • B01J2208/00495Controlling the temperature by thermal insulation means using insulating materials or refractories
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00991Disengagement zone in fluidised-bed reactors

Definitions

  • the present invention relates to the field of chemical engineering reactions.
  • it relates to a split type slurry-bed reaction equipment and a method for conducting a slurry-bed reaction using said equipment.
  • Fischer-Tropsch synthesis technology has attracted much attention for its ability to produce cleaner fuel from carbon and hydrogen containing raw materials, such as coal, natural gas, and biomass.
  • catalysts which are used in liquid fuel production by Fischer-Tropsch synthesis using coal or natural gas as raw materials.
  • One type is iron-based catalysts and the other cobalt-based catalysts.
  • Iron-based catalysts need to be replaced every 70-100 days due to poor stability. The frequent replacement of the catalysts limited the development of this technology. With better stability, cobalt-based catalysts could avoid frequent replacement of the catalysts and be used in Fischer-Tropsch synthesis fixed-bed reactors.
  • a Fischer-Tropsch synthesis reaction is an exothermal reaction.
  • a Fischer-Tropsch synthesis fixed-bed reactor is prone to problems such as hotspot and coking, which make it difficult for amplification.
  • Fischer-Tropsch synthesis reactors have been developed as circulating fluidized beds, fixed fluidized beds and slurry beds later.
  • the fluidization process is hard to control.
  • the utilization rate of catalysts is low with serious attrition, and the production capacity is still low.
  • a fixed fluidized bed has simple structure and can overcome the problems of low catalyst utilization rate and high attrition.
  • it is applied to only high-temperature Fischer-Tropsch synthesis rather than the production of higher value-added heavy fraction such as wax.
  • the gas-liquid-solid three-phase bubbling suspension slurry-bed reactor technology can effectively remove reaction heat and the reaction temperature could still be effectively controlled using a highly active catalyst (i.e. a high yield catalyst), which can facilitate selective synthesis of heavy fraction products and improve the yield of middle fraction products, particularly a diesel.
  • the reaction environment of catalysts can be improved, thus the attrition of catalysts can be decreased.
  • Slurry-bed reactors have advantages in heat control, being relatively easy to amplify and to realize single-series large-scale production.
  • slurry-bed F-T synthesis reactors still involve the integration of multiple key technologies, among which the separation method of entrainment and fine particle entrainment from the tower top tail gas is one of the key technologies.
  • the entrainment in the tail gas at a reactor outlet will lead to high solid content of the downstream condensation products and affect the subsequent processing of the products and operation stability. Such effects are even worse especially when the accumulation of oxygen-containing compounds results too much foam or even flooding at the gas-liquid interface of a reactor.
  • a slurry-bed reaction equipment wherein the separation apparatus is located outside of the reaction apparatus.
  • the separation apparatus is in flow communication with the reaction apparatus and located downstream of the reaction apparatus so that the separated liquid and solid materials from the tail gas would not return to the reaction apparatus.
  • a slurry-bed reaction equipment is provided, wherein the reaction equipment comprises a separation apparatus and a reaction apparatus.
  • the separation apparatus is located outside of the reaction apparatus.
  • the separation apparatus is in flow communication with the reaction apparatus and located downstream of the reaction apparatus, wherein the separation apparatus includes at least one separator and a condensation region. At least a part of the separator is located in the condensation region.
  • the separation apparatus further comprises a separator gas collection chamber and a clean gas collection chamber which are located above the condensation region.
  • the separation apparatus further comprises a liquid-solid materials collection section located below the condensation region.
  • the reaction apparatus comprises a slurry section and a gas phase section, and the slurry section is located below the gas phase section.
  • the reaction apparatus further comprises a heat insulating component.
  • the heat insulating component surrounds the gas phase section and the upper part of the slurry section along the longitudinal direction.
  • the heat insulating component comprises a heating device.
  • the reaction apparatus comprises a flared section comprising the gas phase section and the upper part of the slurry section.
  • Another aspect of the present invention relates to a method for conducting slurry bed reaction using the slurry-bed reaction equipment of the present invention, the method comprises the following steps: feed is fed into the reaction apparatus, contacted with the slurry in the slurry section in the lower part of the reaction apparatus for reaction, the resulting gas materials ascend to the gas phase section in the upper part; the resulting gas materials depart from the upper part of the reaction apparatus and are delivered to the separation apparatus.
  • the resulting gas materials may carry liquid and solid materials and are separated in the separator.
  • the separated gas substance is collected to the clean gas collection chamber.
  • the separated liquid-solid materials are collected to the liquid-solid materials collection section.
  • the gas materials include the resulting gas products from the aforementioned reaction and the unreacted gas raw materials which comprise reacting gases and inert gases.
  • the aforementioned application is a Fischer-Tropsch synthesis reaction, wherein the resulting gas products comprise, for example, lower hydrocarbons such as methane and ethane; the gas raw materials comprise, for example, hydrogen, carbon monoxide, nitrogen, carbon dioxide, etc.
  • the method further comprises cooling the part of the separator located in the condensation section.
  • the part of the separator located in the condensation section is cooled to 50-200 ° C , more preferably 80-180 ° C , most preferably 100-150 ° C .
  • the reaction method further comprises heating and insulating the gas phase section and the upper part of the slurry section.
  • the gas phase section and the upper part of the slurry section are heated and insulated to prevent or reduce condensation of substances such as water vapor in the reaction apparatus.
  • the gas phase section and the upper part of the slurry section are heated and insulated to 210-240 ° C , preferably 215-235 ° C .
  • liquid and solid materials collected in the liquid-solid materials collection section do not return to the reaction apparatus.
  • Another aspect of the present invention provides a method for conducting a slurry-bed reaction using the slurry-bed reaction equipment of the present invention, said method comprises the following steps: feed is fed into the reaction apparatus of the reaction equipment and reacted in the reaction apparatus; the resulting gas materials are transferred from the reaction apparatus to the separation apparatus of the reaction equipment; the gas materials are separated in the separator of the separation equipment so that gas substances are separated from liquid-solid substances in the gas materials, wherein at least a portion of the separator is cooled to facilitate the separation of the gas substances and the liquid-solid substances.
  • the upper part of the reaction apparatus is heated and insulated to prevent substances condensation in the reaction apparatus.
  • the temperature of the heating and insulating is at 210-240 ° C , preferably 215-235 ° C .
  • Figure 1 is the scheme of the slurry-bed reaction equipment of the present invention.
  • FIG. 1 is the detailed structure of the separation apparatus.
  • the “range” disclosed herein is in the form of lower limit and upper limit. There can be one or more lower limits, and one or more upper limits, respectively. A given range is limited by selecting a lower limit and an upper limit. The selected lower limit and upper limit will determine the boundary of the specific range. The range limited by such way can be included or combined, i.e. any lower limit and any upper limit can be combined to form a range.
  • the range of "60-120 and 80-1 10" that is given by specific parameters can be understood to be 60-80, 60-1 10, 80-120 and 1 10-120.
  • step (a) and (b) means said method can comprise steps (a) and (b) in such order, or steps (b) and (a) in such order.
  • said method further comprising step (c) means step (c) can be added into said method in any order, for example, said method may comprise steps such as steps (a), (b) and (c), or steps (a), (c) and (b), or steps (c), (a) and (b).
  • Figure 1 shows a s slurry-bed reaction equipment of the present invention, mainly comprising reaction apparatus 101 and separation apparatus 6.
  • the separation apparatus 6 is located outside of the reaction apparatus 101 and is in flow communication with the reaction apparatus 101 and located downstream of the reaction apparatus 101, such that the liquid (such as water) and solid materials (such as catalyst particles) separated from the tail gas would not get back to the slurry bed of the reaction apparatus, thereby avoiding problems in the art that the condensation of byproducts (e.g. water vapor or hydrocarbons components) in the reaction apparatus poisons the catalyst and inactivates the catalyst powder.
  • byproducts e.g. water vapor or hydrocarbons components
  • the reaction equipment of the present invention is especially suitable for slurry-bed Fischer-Tropsch reaction system for synthesis gas, to prevent the byproduct of water vapor from condensing and getting back to the reaction system which will poison cobalt-based or iron-based catalysts, and to prevent the inactivation of these catalyst powder.
  • the detailed description is also discussed hereinafter in combination with the reaction process.
  • the reaction equipment of the present invention is suitable not only for the slurry-bed Fischer-Tropsch reaction system of synthesis gas, but also for any other slurry-bed reaction system which need to prevent the liquid and solid materials carried in the tail gas from getting back to the slurry bed.
  • Figure 1 only shows the essential constitute components of the reaction equipment, however, various other means and components can also be added according to a specific process.
  • the Fischer-Tropsch reaction when the Fischer-Tropsch reaction is conducted in the reaction equipment of the present invention using synthesis gas as raw materials, cobalt-based or iron-based catalyst solid particles are suspended in a hydrocarbon oil or heavy wax solvent, the resulting solid-liquid slurry is contained in the slurry section 1 of the reaction apparatus.
  • the Fischer-Tropsch reaction and associated catalyst system are well-known in the art.
  • the raw synthesis gas is introduced into the reactor from the lower part of the reaction equipment and ascend through the slurry.
  • the inlet of the reaction apparatus is not limited to be at the lower part of the reaction apparatus.
  • the reaction apparatus may also comprise a gas distributor provided at the bottom of the reaction apparatus so that the raw synthesis gas, before contacting with the slurry, can flow into the reaction apparatus uniformly by getting through the gas distributor .
  • the gas distributor can be any kind of gas distributor known in the art or will be developed in the future, for example, plate with hole or nozzle structures.
  • Heat exchanger and liquid product extraction components can be provided optionally in the slurry section 1.
  • the heat exchanger can be any shape of pipe, plate or grate that allows any conventional heat exchange medium, for example air, water, organic solvent, supercritical fluid to flow therethrough and provide heating or cooling to the slurry such that the temperature in the reaction apparatus can be maintained within a desired range.
  • the temperature of the slurry section in the reaction apparatus is 200-280 ° C , preferably 210-260 ° C , more preferably 220-240 ° C .
  • the pressure in the reaction apparatus is l-8MPa, preferably 2-6MPa, more preferably 2-4MPa.
  • a skilled person in the art can employ other temperature and pressure conditions according to requirements of a specific mechanism and process when conducting other reactions in the reaction apparatus.
  • the ascending synthesis gas contacts with the catalyst particles in the slurry and reacts to generate hydrocarbon products having a range of carbon atoms, byproducts of light hydrocarbon, carbon mono-oxide, carbon dioxide, methane, water vapor from dehydration reactions, and unreacted synthesis gas, which ascend from the slurry section 1 as tail gas to the gas phase section 2.
  • the majority of heavy hydrocarbon products dissolve in the slurry and are extracted outside the reactor after being filtrated by the liquid-solid separation system in the reactor, and are subject to further post-treatment processing.
  • the tail gas also carries materials that are prone to condensation, such as water vapor and hydrocarbon, and catalyst solid that is prone to sedimentation.
  • the reaction apparatus can optionally comprise a flared section.
  • the diameter of the reaction apparatus increases in the flared section.
  • the flared section can comprise the upper part of the slurry section and the entire gas phase section.
  • the quality and thickness of the wall material of the flared section can withstand a reaction temperature and pressure. Possible entrainment is reduced by the flared section through reducing the ascending rate of the tail gas.
  • a foam eliminator can be optionally provided in the flared section depending on the circulating ratio of the tail gas to the fresh feed synthesis gas in the slurry-bed reaction system, and the apparent operating gas velocity in the tower.
  • the gas flow velocity in the flared section is within a range of 0.01 ⁇ 0.25m/s, preferably 0.1 ⁇ 0.2m/s, by adjusting the pressure and slurry quantity in the reaction apparatus and the flow velocity of the raw synthesis gas at the bottom inlet.
  • the tail gas will carry a large quantity of droplets or catalyst particles and subsequent processing equipment or pipeline will possibly be clogged if the gas flow velocity is too high.
  • the flared section will be bulky and affect the manufacture and installation of the equipment.
  • a heat insulating component 4 is arranged around the reaction apparatus over the entire flared section.
  • the heating insulating component 4 comprises a heating device.
  • the heat insulating component 4 is needed to keep warm of and heat the reaction apparatus, so that the gas phase section 2 can be maintained at a specific temperature and prevent the water vapor and/or hydrocarbon components carried in the tail gas ascending in the gas phase space from condensing and dropping back to the lower slurry.
  • the temperature of the gas phase section 2 and the upper part of the slurry section 1 is maintained by the heat insulating component 4 within 210-240 ° C , preferably 215-235 ° C for aforementioned purpose.
  • the tail gas 5 carrying entrainment departs from the reaction apparatus without condensation or sedimentation and is delivered to the separation apparatus 6 located downstream.
  • the arrow near the number 5 in the Figure 1 shows the direction of the tail gas flow.
  • Figure 2 shows details of the separation apparatus of the present invention.
  • the separation apparatus 6 mainly comprises separator 1 1 , and clean gas collection chamber 14, separator gas collection chamber 12, condensation section 15 and liquid-solid materials collection section 17.
  • the separator gas collection chamber 12, clean gas collection chamber 14 are provided sequentially from top to bottom.
  • Separator gas collection chamber 12, clean gas collection chamber 14, condensation section 15 and liquid-solid materials collection section 17 are separate from each other. At least a part of the separator 1 1 is located in the condensation section 15.
  • the clean gas collection chamber 14 and the separator gas collection chamber 12 are separated by a separation component 122 which is connected with the top part of the separator 1 1 and the inner wall of the separation apparatus 6 in a sealed manner to prevent the tail gas 5 carrying entrainments from entering into the clean gas collection chamber 14.
  • the separator gas collection chamber 12 and the condensation section 15 are separated by a separation component 124 which is connected with the middle part of the separator 1 1 and the inner wall of the separation apparatus 6 in a sealed manner to prevent the tail gas carrying entrainments from going down into the condensation section 15, meanwhile the cooling medium in the condensation section 15 will not flow upwards into the separator gas collection chamber 12.
  • the condensation section 15 and the liquid-solid materials collection section are separated by a separation component 126, which is connected with the lower part of the separator 1 1 and the inner wall of the separation apparatus 6 in a sealed manner to prevent the cooling medium 9 that is fed into the condensation section 15 from flowing down into the liquid - solid materials collection section 17, meanwhile the substances within the liquid - solid materials collection section 17 will not go up into the condensation section 15.
  • the separation components 122, 124 and 126 may be a metal or non-metal material, such as a separator or a baffle etc.
  • the separation components can be separate components or integrate with other components. Furthermore, the separation components can be provided in the horizontal position as shown in Figure 2, or be provided obliquely as long as it can achieve the separation effects of the present invention.
  • the separator 1 1 is preferably a cyclone separator. Any other suitable separator that can be used for solid-liquid separation or gas-liquid-solid separation can also be used.
  • the separation apparatus use multiple separators 1 1 provided in parallel, for example 2-50 separators.
  • the separation apparatus comprises multiple vertical parallel cyclone separators. At least a part of these cyclone separators is located in the condensation section 15 and is condensed. Separation is conducted by the vertically installed cyclone separator through rotation speed difference and the density difference of the two phases under centrifugal force and gravity, the separation effect of the cyclone separator is far better than that of common gas-liquid separation tank.
  • the separation effect of the cyclone separator is further enhanced as a result of condensation in the condensation section 15.
  • the cyclone separator and the condensation section 15 constitute an integrated equipment.
  • the tail gas 5 carrying entrainment gets in the separator gas collection chamber 12 and then gets in each cyclone separator from one or more cyclone separator inlets 13, preferably gets in each cyclone separator along the tangential direction.
  • the gaseous tail gas is separated under centrifugal force and gravity in the cyclone separator. Also separated is a slurry phase containing condensed water, heavy distillate oil and catalyst particles.
  • the cooling medium is introduced into the condensation section 15 through the cooling medium inlet 127 as indicated by arrow 9 and cools the part of the separator 1 1 located in the condensation section 15 so that the water vapor and heavy distillate oil in the tail gas can condense in the separator simultaneously.
  • the density difference between the gas phase and slurry phase is therefore increased and the cyclone separation effect is enhanced.
  • the cooling medium is then extracted from the cooling medium outlet 128 as indicated by arrow 10 to an external circulating equipment.
  • the cooling medium can be any cooling medium commonly used in the art, for example, cooling water, halohydrocarbon, liquid ammonia, ammonia water or cold raw synthesis gas.
  • the position of the cooling medium inlet 127 and the cooling medium outlet 128 can be different for different cooling media.
  • the cooling medium inlet is in the upper region of the condensation section, and the cooling medium outlet is in the lower region of the condensation section.
  • the cooling medium inlet 127 is in the lower region of the condensation section 15, and the cooling medium outlet 128 is in the upper region of the condensation section 15.
  • the separator is preferably maintained by the cooling medium at the temperature of 5-200 ° C , preferably 80-180 ° C , more preferably 100-150 ° C .
  • the condensation section 15 can be cooled by any suitable mechanism, such as a heat exchange circulating mechanism or shell-and-tube cooling mechanism.
  • the condensation section 15 may use any conventional heat exchange circulating mechanism, for example, pipelines can be provided therein to let cooling medium flow through.
  • the condensation section 15 together with separator 1 1 can constitute shell-and-tube cooling mechanism, which means that the condensation section 15 is a container while a part of the separator 1 1 goes through the container.
  • the cooling medium flows in from the cooling medium inlet 127 in the lower part of the condensation section 15 and flows out from the cooling medium outlet 128 in the upper part, thereby cooling the materials in the separator 1 1.
  • the tail gas is delivered upwardly to the clean gas collection chamber 14.
  • the cleaned tail gas 7 is delivered to the outside of the reaction equipment for further processing.
  • the condensate water, heavy fraction and catalyst particles are separated as a slurry and descend from the lower outlet of the cyclone separator and are collected in the liquid-solid materials collection section.
  • the height of the gas-liquid interface 16 is measured from time to time by the operator in an automatic or manual manner.
  • the slurry is expelled from the separation apparatus in an intermittent or continuous manner to ensure that the height of the gas-liquid interface 16 is within a reasonable range.
  • the separation apparatus of the present invention is located outside of the reaction apparatus, and the separation apparatus is in communication with the reaction apparatus and located downstream of the reaction apparatus.
  • the separation apparatus and reaction apparatus are provided separate from each other in the present invention.
  • a heat insulating component is provided in the gas phase section space in the upper part of the slurry bed in the reaction equipment to ensure the water vapor would not condense in the reaction equipment and get back to the slurry, which will result inactivation of the catalyst. Also, gas-liquid separation is not conducted in the reaction equipment so as to prevent the solid catalyst carried in the tail gas from getting back to the slurry and then causing pulverization and inactivation of the catalyst particles.

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

Abstract

A slurry-bed reaction equipment comprises a reaction apparatus (101) and a separation apparatus (6) located outside of the reaction apparatus (101). The separation apparatus (6) is in flow communication with the reaction apparatus (101) and located downstream of the reaction apparatus (101). The separation apparatus (6) includes at least one separator (11) and a condensation region (15), and at least a part of the separator (11) is located in the condensation region (15) for enhancing the separation by condensation. A method for conducting a slurry-bed reaction using the reaction equipment is also provided.

Description

SLURRY-BED REACTION EQUIPMENT AND USAGE THEREOF
The field of the Invention
The present invention relates to the field of chemical engineering reactions. In particular, it relates to a split type slurry-bed reaction equipment and a method for conducting a slurry-bed reaction using said equipment.
Background
With oil resources decreasing worldwide, development of alternative energy technology has been paid more and more attention, among which Fischer-Tropsch synthesis technology has attracted much attention for its ability to produce cleaner fuel from carbon and hydrogen containing raw materials, such as coal, natural gas, and biomass.
There are two types of catalysts which are used in liquid fuel production by Fischer-Tropsch synthesis using coal or natural gas as raw materials. One type is iron-based catalysts and the other cobalt-based catalysts. Iron-based catalysts need to be replaced every 70-100 days due to poor stability. The frequent replacement of the catalysts limited the development of this technology. With better stability, cobalt-based catalysts could avoid frequent replacement of the catalysts and be used in Fischer-Tropsch synthesis fixed-bed reactors. However, a Fischer-Tropsch synthesis reaction is an exothermal reaction. A Fischer-Tropsch synthesis fixed-bed reactor is prone to problems such as hotspot and coking, which make it difficult for amplification. Fischer-Tropsch synthesis reactors have been developed as circulating fluidized beds, fixed fluidized beds and slurry beds later. However, in a circulating fluidized bed, the fluidization process is hard to control. The utilization rate of catalysts is low with serious attrition, and the production capacity is still low. A fixed fluidized bed has simple structure and can overcome the problems of low catalyst utilization rate and high attrition. However, it is applied to only high-temperature Fischer-Tropsch synthesis rather than the production of higher value-added heavy fraction such as wax. Compared with conventional fluidized bed reactors, the gas-liquid-solid three-phase bubbling suspension slurry-bed reactor technology can effectively remove reaction heat and the reaction temperature could still be effectively controlled using a highly active catalyst (i.e. a high yield catalyst), which can facilitate selective synthesis of heavy fraction products and improve the yield of middle fraction products, particularly a diesel. In addition, the reaction environment of catalysts can be improved, thus the attrition of catalysts can be decreased.
Slurry-bed reactors have advantages in heat control, being relatively easy to amplify and to realize single-series large-scale production. However, slurry-bed F-T synthesis reactors still involve the integration of multiple key technologies, among which the separation method of entrainment and fine particle entrainment from the tower top tail gas is one of the key technologies. The entrainment in the tail gas at a reactor outlet will lead to high solid content of the downstream condensation products and affect the subsequent processing of the products and operation stability. Such effects are even worse especially when the accumulation of oxygen-containing compounds results too much foam or even flooding at the gas-liquid interface of a reactor. There is still no method to solve the entrainment problem systematically. Therefore, a new slurry-bed reactor and method to solve the above problems are desired.
Summery of the Invention
To solve the aforementioned issues, the applicant has developed a slurry-bed reaction equipment, wherein the separation apparatus is located outside of the reaction apparatus. The separation apparatus is in flow communication with the reaction apparatus and located downstream of the reaction apparatus so that the separated liquid and solid materials from the tail gas would not return to the reaction apparatus. In particular, in one aspect of the present invention, a slurry-bed reaction equipment is provided, wherein the reaction equipment comprises a separation apparatus and a reaction apparatus. The separation apparatus is located outside of the reaction apparatus. The separation apparatus is in flow communication with the reaction apparatus and located downstream of the reaction apparatus, wherein the separation apparatus includes at least one separator and a condensation region. At least a part of the separator is located in the condensation region. In a preferred embodiment, the separation apparatus further comprises a separator gas collection chamber and a clean gas collection chamber which are located above the condensation region. In another preferred embodiment, the separation apparatus further comprises a liquid-solid materials collection section located below the condensation region.
In an embodiment of the present invention, the reaction apparatus comprises a slurry section and a gas phase section, and the slurry section is located below the gas phase section.
In an embodiment of the present invention, the reaction apparatus further comprises a heat insulating component. The heat insulating component surrounds the gas phase section and the upper part of the slurry section along the longitudinal direction. Preferably, the heat insulating component comprises a heating device.
In an embodiment of the present invention, the reaction apparatus comprises a flared section comprising the gas phase section and the upper part of the slurry section.
Another aspect of the present invention relates to a method for conducting slurry bed reaction using the slurry-bed reaction equipment of the present invention, the method comprises the following steps: feed is fed into the reaction apparatus, contacted with the slurry in the slurry section in the lower part of the reaction apparatus for reaction, the resulting gas materials ascend to the gas phase section in the upper part; the resulting gas materials depart from the upper part of the reaction apparatus and are delivered to the separation apparatus. The resulting gas materials may carry liquid and solid materials and are separated in the separator. The separated gas substance is collected to the clean gas collection chamber. The separated liquid-solid materials are collected to the liquid-solid materials collection section. The gas materials include the resulting gas products from the aforementioned reaction and the unreacted gas raw materials which comprise reacting gases and inert gases. In an embodiment of the present invention, the aforementioned application is a Fischer-Tropsch synthesis reaction, wherein the resulting gas products comprise, for example, lower hydrocarbons such as methane and ethane; the gas raw materials comprise, for example, hydrogen, carbon monoxide, nitrogen, carbon dioxide, etc. In an embodiment of the present invention, the method further comprises cooling the part of the separator located in the condensation section. Preferably, the part of the separator located in the condensation section is cooled to 50-200 °C , more preferably 80-180°C , most preferably 100-150°C . In another embodiment of the present invention, the reaction method further comprises heating and insulating the gas phase section and the upper part of the slurry section. The gas phase section and the upper part of the slurry section are heated and insulated to prevent or reduce condensation of substances such as water vapor in the reaction apparatus. Preferably, the gas phase section and the upper part of the slurry section are heated and insulated to 210-240 °C , preferably 215-235 °C .
In another embodiment of the present invention, the liquid and solid materials collected in the liquid-solid materials collection section do not return to the reaction apparatus.
Another aspect of the present invention provides a method for conducting a slurry-bed reaction using the slurry-bed reaction equipment of the present invention, said method comprises the following steps: feed is fed into the reaction apparatus of the reaction equipment and reacted in the reaction apparatus; the resulting gas materials are transferred from the reaction apparatus to the separation apparatus of the reaction equipment; the gas materials are separated in the separator of the separation equipment so that gas substances are separated from liquid-solid substances in the gas materials, wherein at least a portion of the separator is cooled to facilitate the separation of the gas substances and the liquid-solid substances. In an embodiment, the upper part of the reaction apparatus is heated and insulated to prevent substances condensation in the reaction apparatus. Preferably, the temperature of the heating and insulating is at 210-240 °C , preferably 215-235°C .
Brief Description of the Drawings
The preferred embodiment of the present invention will be set forth in combination with the drawings.
Figure 1 is the scheme of the slurry-bed reaction equipment of the present invention.
Figure 2 is the detailed structure of the separation apparatus.
The components represented by reference labels in drawings are as follows:
1 Slurry section
2 Gas phase section
3 Slurry-gas phase interface
4 Heat insulating component
5 Tail gas carrying entrainment
6 Separation apparatus 7 Cleaned tail gas
8 Separated liquid and solid materials
9 Arrow (indicating direction that Cooling medium flows in)
10 Arrow (indicating direction that Cooling medium flows out)
1 1 Separator
12 Separator gas collection chamber
13 Separator inlet
14 Clean gas collection chamber
15 Condensation section
16 Gas-liquid interface
17 Liquid-solid materials collection section
101 Reaction apparatus
122, 124, 126 Separation components
127 Cooling medium inlet
128 Cooling medium outlet
Detail Description of the Invention
The "range" disclosed herein is in the form of lower limit and upper limit. There can be one or more lower limits, and one or more upper limits, respectively. A given range is limited by selecting a lower limit and an upper limit. The selected lower limit and upper limit will determine the boundary of the specific range. The range limited by such way can be included or combined, i.e. any lower limit and any upper limit can be combined to form a range. For example, the range of "60-120 and 80-1 10" that is given by specific parameters can be understood to be 60-80, 60-1 10, 80-120 and 1 10-120. In addition, if the minimum value is 1 and 2, and a maximum value is 3, 4, and 5, the following range can thus be expected: 1-2, 1-3, 1-4, 1-5, 2-3, 2-4, 2-5, 3-4, 3-5 and 4-5. Unless otherwise specified, all of the embodiments and preferred embodiments described herein can be combined to obtain new technical solutions. Unless otherwise specified, all of the technical features and preferred features described herein can be combined to obtain new technical solutions.
Unless otherwise specified, all of the steps described herein can be performed in order or randomly, preferably in order. For example, said method comprises steps (a) and (b) means said method can comprise steps (a) and (b) in such order, or steps (b) and (a) in such order. For example, said method further comprising step (c) means step (c) can be added into said method in any order, for example, said method may comprise steps such as steps (a), (b) and (c), or steps (a), (c) and (b), or steps (c), (a) and (b). Some preferred embodiments of the present invention will be discussed hereinafter in combination with the drawings. A person skilled in the art can understand that various equivalent alternations, modifications and combinations may be made to these embodiments without departing from the scope limited by the claims of the present invention. New technical solutions obtained by above-referenced alternations, modifications and combinations are within the scope of the present invention.
Figure 1 shows a s slurry-bed reaction equipment of the present invention, mainly comprising reaction apparatus 101 and separation apparatus 6. The separation apparatus 6 is located outside of the reaction apparatus 101 and is in flow communication with the reaction apparatus 101 and located downstream of the reaction apparatus 101, such that the liquid (such as water) and solid materials (such as catalyst particles) separated from the tail gas would not get back to the slurry bed of the reaction apparatus, thereby avoiding problems in the art that the condensation of byproducts (e.g. water vapor or hydrocarbons components) in the reaction apparatus poisons the catalyst and inactivates the catalyst powder. The reaction equipment of the present invention is especially suitable for slurry-bed Fischer-Tropsch reaction system for synthesis gas, to prevent the byproduct of water vapor from condensing and getting back to the reaction system which will poison cobalt-based or iron-based catalysts, and to prevent the inactivation of these catalyst powder. The detailed description is also discussed hereinafter in combination with the reaction process. However, it should be understood that the reaction equipment of the present invention is suitable not only for the slurry-bed Fischer-Tropsch reaction system of synthesis gas, but also for any other slurry-bed reaction system which need to prevent the liquid and solid materials carried in the tail gas from getting back to the slurry bed. Figure 1 only shows the essential constitute components of the reaction equipment, however, various other means and components can also be added according to a specific process.
As shown in Figure 1 , when the Fischer-Tropsch reaction is conducted in the reaction equipment of the present invention using synthesis gas as raw materials, cobalt-based or iron-based catalyst solid particles are suspended in a hydrocarbon oil or heavy wax solvent, the resulting solid-liquid slurry is contained in the slurry section 1 of the reaction apparatus. The Fischer-Tropsch reaction and associated catalyst system are well-known in the art. The raw synthesis gas is introduced into the reactor from the lower part of the reaction equipment and ascend through the slurry. The inlet of the reaction apparatus is not limited to be at the lower part of the reaction apparatus. Further, the reaction apparatus may also comprise a gas distributor provided at the bottom of the reaction apparatus so that the raw synthesis gas, before contacting with the slurry, can flow into the reaction apparatus uniformly by getting through the gas distributor . The gas distributor can be any kind of gas distributor known in the art or will be developed in the future, for example, plate with hole or nozzle structures. Heat exchanger and liquid product extraction components can be provided optionally in the slurry section 1. The heat exchanger can be any shape of pipe, plate or grate that allows any conventional heat exchange medium, for example air, water, organic solvent, supercritical fluid to flow therethrough and provide heating or cooling to the slurry such that the temperature in the reaction apparatus can be maintained within a desired range. In a preferred embodiment, for the Fischer-Tropsch reaction, the temperature of the slurry section in the reaction apparatus is 200-280 °C , preferably 210-260 °C , more preferably 220-240 °C . The pressure in the reaction apparatus is l-8MPa, preferably 2-6MPa, more preferably 2-4MPa. A skilled person in the art can employ other temperature and pressure conditions according to requirements of a specific mechanism and process when conducting other reactions in the reaction apparatus.
The ascending synthesis gas contacts with the catalyst particles in the slurry and reacts to generate hydrocarbon products having a range of carbon atoms, byproducts of light hydrocarbon, carbon mono-oxide, carbon dioxide, methane, water vapor from dehydration reactions, and unreacted synthesis gas, which ascend from the slurry section 1 as tail gas to the gas phase section 2. The majority of heavy hydrocarbon products dissolve in the slurry and are extracted outside the reactor after being filtrated by the liquid-solid separation system in the reactor, and are subject to further post-treatment processing. Besides uncondensed gas components, the tail gas also carries materials that are prone to condensation, such as water vapor and hydrocarbon, and catalyst solid that is prone to sedimentation. The reaction apparatus can optionally comprise a flared section. In particular, the diameter of the reaction apparatus increases in the flared section. The flared section can comprise the upper part of the slurry section and the entire gas phase section. The quality and thickness of the wall material of the flared section can withstand a reaction temperature and pressure. Possible entrainment is reduced by the flared section through reducing the ascending rate of the tail gas. In addition, a foam eliminator can be optionally provided in the flared section depending on the circulating ratio of the tail gas to the fresh feed synthesis gas in the slurry-bed reaction system, and the apparent operating gas velocity in the tower. In a preferred embodiment, the gas flow velocity in the flared section is within a range of 0.01~0.25m/s, preferably 0.1~0.2m/s, by adjusting the pressure and slurry quantity in the reaction apparatus and the flow velocity of the raw synthesis gas at the bottom inlet. The tail gas will carry a large quantity of droplets or catalyst particles and subsequent processing equipment or pipeline will possibly be clogged if the gas flow velocity is too high. However, if the gas flow velocity is too slow, the flared section will be bulky and affect the manufacture and installation of the equipment. In a preferred embodiment of the present invention, a heat insulating component 4 is arranged around the reaction apparatus over the entire flared section. Preferably, the heating insulating component 4 comprises a heating device. Since the exothermal reaction no longer takes place in the gas phase section, the heat insulating component 4 is needed to keep warm of and heat the reaction apparatus, so that the gas phase section 2 can be maintained at a specific temperature and prevent the water vapor and/or hydrocarbon components carried in the tail gas ascending in the gas phase space from condensing and dropping back to the lower slurry. The temperature of the gas phase section 2 and the upper part of the slurry section 1 is maintained by the heat insulating component 4 within 210-240 °C , preferably 215-235 °C for aforementioned purpose.
The tail gas 5 carrying entrainment departs from the reaction apparatus without condensation or sedimentation and is delivered to the separation apparatus 6 located downstream. The arrow near the number 5 in the Figure 1 shows the direction of the tail gas flow. Figure 2 shows details of the separation apparatus of the present invention. The separation apparatus 6 mainly comprises separator 1 1 , and clean gas collection chamber 14, separator gas collection chamber 12, condensation section 15 and liquid-solid materials collection section 17. The separator gas collection chamber 12, clean gas collection chamber 14 are provided sequentially from top to bottom. Separator gas collection chamber 12, clean gas collection chamber 14, condensation section 15 and liquid-solid materials collection section 17 are separate from each other. At least a part of the separator 1 1 is located in the condensation section 15. The clean gas collection chamber 14 and the separator gas collection chamber 12 are separated by a separation component 122 which is connected with the top part of the separator 1 1 and the inner wall of the separation apparatus 6 in a sealed manner to prevent the tail gas 5 carrying entrainments from entering into the clean gas collection chamber 14. The separator gas collection chamber 12 and the condensation section 15 are separated by a separation component 124 which is connected with the middle part of the separator 1 1 and the inner wall of the separation apparatus 6 in a sealed manner to prevent the tail gas carrying entrainments from going down into the condensation section 15, meanwhile the cooling medium in the condensation section 15 will not flow upwards into the separator gas collection chamber 12. The condensation section 15 and the liquid-solid materials collection section are separated by a separation component 126, which is connected with the lower part of the separator 1 1 and the inner wall of the separation apparatus 6 in a sealed manner to prevent the cooling medium 9 that is fed into the condensation section 15 from flowing down into the liquid - solid materials collection section 17, meanwhile the substances within the liquid - solid materials collection section 17 will not go up into the condensation section 15. The separation components 122, 124 and 126 may be a metal or non-metal material, such as a separator or a baffle etc. The separation components can be separate components or integrate with other components. Furthermore, the separation components can be provided in the horizontal position as shown in Figure 2, or be provided obliquely as long as it can achieve the separation effects of the present invention. The separator 1 1 is preferably a cyclone separator. Any other suitable separator that can be used for solid-liquid separation or gas-liquid-solid separation can also be used. In a preferred embodiment of the present invention, the separation apparatus use multiple separators 1 1 provided in parallel, for example 2-50 separators. In a most preferred embodiment, the separation apparatus comprises multiple vertical parallel cyclone separators. At least a part of these cyclone separators is located in the condensation section 15 and is condensed. Separation is conducted by the vertically installed cyclone separator through rotation speed difference and the density difference of the two phases under centrifugal force and gravity, the separation effect of the cyclone separator is far better than that of common gas-liquid separation tank. The separation effect of the cyclone separator is further enhanced as a result of condensation in the condensation section 15. In a preferred embodiment of the present invention, the cyclone separator and the condensation section 15 constitute an integrated equipment. The tail gas 5 carrying entrainment gets in the separator gas collection chamber 12 and then gets in each cyclone separator from one or more cyclone separator inlets 13, preferably gets in each cyclone separator along the tangential direction. The gaseous tail gas is separated under centrifugal force and gravity in the cyclone separator. Also separated is a slurry phase containing condensed water, heavy distillate oil and catalyst particles. In the separation process, the cooling medium is introduced into the condensation section 15 through the cooling medium inlet 127 as indicated by arrow 9 and cools the part of the separator 1 1 located in the condensation section 15 so that the water vapor and heavy distillate oil in the tail gas can condense in the separator simultaneously. The density difference between the gas phase and slurry phase is therefore increased and the cyclone separation effect is enhanced. The cooling medium is then extracted from the cooling medium outlet 128 as indicated by arrow 10 to an external circulating equipment. The cooling medium can be any cooling medium commonly used in the art, for example, cooling water, halohydrocarbon, liquid ammonia, ammonia water or cold raw synthesis gas. The position of the cooling medium inlet 127 and the cooling medium outlet 128 can be different for different cooling media. In an embodiment, the cooling medium inlet is in the upper region of the condensation section, and the cooling medium outlet is in the lower region of the condensation section. Preferably, in the embodiment shown in Figure 2, the cooling medium inlet 127 is in the lower region of the condensation section 15, and the cooling medium outlet 128 is in the upper region of the condensation section 15. To ensure the cooling effect, the separator is preferably maintained by the cooling medium at the temperature of 5-200 °C , preferably 80-180°C , more preferably 100-150°C . The condensation section 15 can be cooled by any suitable mechanism, such as a heat exchange circulating mechanism or shell-and-tube cooling mechanism. The condensation section 15 may use any conventional heat exchange circulating mechanism, for example, pipelines can be provided therein to let cooling medium flow through. Alternatively, the condensation section 15 together with separator 1 1 can constitute shell-and-tube cooling mechanism, which means that the condensation section 15 is a container while a part of the separator 1 1 goes through the container. The cooling medium flows in from the cooling medium inlet 127 in the lower part of the condensation section 15 and flows out from the cooling medium outlet 128 in the upper part, thereby cooling the materials in the separator 1 1. After the liquid and solid materials are removed from the tail gas in the cyclone separator, the tail gas is delivered upwardly to the clean gas collection chamber 14. The cleaned tail gas 7 is delivered to the outside of the reaction equipment for further processing. The condensate water, heavy fraction and catalyst particles are separated as a slurry and descend from the lower outlet of the cyclone separator and are collected in the liquid-solid materials collection section. In the reaction process, the height of the gas-liquid interface 16 is measured from time to time by the operator in an automatic or manual manner. The slurry is expelled from the separation apparatus in an intermittent or continuous manner to ensure that the height of the gas-liquid interface 16 is within a reasonable range.
The majority of catalyst particles carried in the tail gas, together with condensate water and heavy fraction rotationally flow and fall down to the bottom liquid-solid materials collection section under centrifugal force and gravity, which can prevent the solid particles from sedimenting and blocking at places such as the subsequent tail gas processing equipment and gas pipeline valves.
The separation apparatus of the present invention is located outside of the reaction apparatus, and the separation apparatus is in communication with the reaction apparatus and located downstream of the reaction apparatus. The separation apparatus and reaction apparatus are provided separate from each other in the present invention.
In a preferred embodiment, a heat insulating component is provided in the gas phase section space in the upper part of the slurry bed in the reaction equipment to ensure the water vapor would not condense in the reaction equipment and get back to the slurry, which will result inactivation of the catalyst. Also, gas-liquid separation is not conducted in the reaction equipment so as to prevent the solid catalyst carried in the tail gas from getting back to the slurry and then causing pulverization and inactivation of the catalyst particles.

Claims

What is claimed is:
1. A slurry-bed reaction equipment, which comprises a reaction apparatus and a separation apparatus, wherein the separation apparatus is located outside of the reaction apparatus, the separation apparatus is in flow communication with the reaction apparatus and located downstream of the reaction apparatus, and the separation apparatus includes at least one separator and a condensation region, wherein at least a part of the separator is located in the condensation region.
2. The slurry-bed reaction equipment of claim 1, wherein the separation apparatus (6) further comprises a separator gas collection chamber (12) and a clean gas collection chamber (14) which are located above the condensation region.
3. The slurry-bed reaction equipment of claim 2, wherein the separation apparatus (6) further comprises a liquid-solid materials collection section (17) located below the condensation region.
4. The slurry-bed reaction equipment of any of claims 1-3, wherein the reaction apparatus (101) comprises a slurry section (1) and a gas phase section (2), and the slurry section (1) is located below the gas phase section (2).
5. The slurry-bed reaction equipment of claim 4, wherein the condensation section (15) comprises a heat exchange circulating structure or shell-and-tube cooling mechanism.
6. The slurry-bed reaction equipment of claim 4, wherein the separator (1 1) includes a gas-liquid separator or a gas-liquid-solid separator, preferably a cyclone separator.
7. The slurry-bed reaction equipment of claim 4, wherein the reaction apparatus (101) further comprises a heat insulating component (4) surrounding the gas phase section (2) and the upper part of the slurry section (1) along the longitudinal direction.
8. The slurry-bed reaction equipment of claim 7, wherein the heat insulating component comprises a heating device.
9. The slurry-bed reaction equipment of claim 4, wherein the reaction apparatus (101) comprises a flared section comprising the gas phase section (2) and the upper part of the slurry section ( 1 ).
10. A method for conducting a slurry-bed reaction using the slurry-bed reaction equipment of any of claims 1-9, said method comprises the following steps:
feed is fed into the reaction apparatus (101), contacted with the slurry in the slurry section (1) in the lower part of the reaction apparatus for reaction, the resulting gas materials ascend to the gas phase section (2) in the upper part;
the resulting gas materials depart from the upper part of the reaction apparatus (101) and are delivered to the separation apparatus (6), the resulting gas materials carrying liquid and solid materials;
the resulting gas materials are separated in the separator (1 1), the separated gas substance is collected to the clean gas collection chamber (14), the separated liquid-solid materials are collected to the liquid-solid materials collection section (17).
1 1. The method of claim 10, wherein the method further comprises cooling the part of the separator (1 1) located in the condensation section (15).
12. The method of claim 1 1, wherein the part of the separator located condensation section is cooled down to 50-200 °C , preferably 80-180°C , more preferably 100-150°C .
13. The method of claim 10, wherein the gas phase section (2) and the upper part of the slurry section (1) are heated and insulated.
14. The method of claim 13, wherein the gas phase section (2) and the upper part of the slurry section (1) are heated and insulated to prevent or reduce substances condensation in the reaction apparatus.
15. The method of claim 13, wherein the gas phase section (2) and the upper part of the slurry section (1) are heated and insulated to 210-240 °C , preferably 215-235°C .
16. The method of claim 10, wherein the liquid-solid materials collected in the liquid-solid materials collection section (17) are not recycled back to the reaction apparatus.
17. A method for conducting a slurry-bed reaction using the slurry-bed reaction equipment of claim 1, said method comprises the following steps:
feed is fed into the reaction apparatus of the reaction equipment and reacted in the reaction apparatus;
the resulting gas materials are transferred from the reaction apparatus to the separation apparatus of the reaction equipment;
the gas materials are separated in the separator of the separation equipment so that gas substances are separated from liquid-solid substances in the gas materials, wherein at least a portion of the separator is cooled to facilitate the separation of the gas substances and liquid-solid substances.
18. The method of claim 17, wherein the upper part of the reaction apparatus is heated and insulated to prevent substances condensation in the reaction apparatus.
19. The method of claim 18, wherein the temperature of the heating and insulating is controlled at 210-240 °C , preferably 215-235 °C .
PCT/CN2014/071647 2013-02-05 2014-01-28 Slurry-bed reaction equipment and usage thereof WO2014121718A1 (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3962070A (en) * 1972-01-03 1976-06-08 Hydrocarbon Research, Inc. H-coal process: slurry oil recycle system
US6822006B1 (en) * 2003-07-02 2004-11-23 Chevron U.S.A. Inc. Methods of controlling the temperature of an exothermic reaction
JP2006022283A (en) * 2004-07-09 2006-01-26 Nippon Steel Corp Slurry bed reaction system for bubbling tower type fisher-tropsh synthesis
WO2010052397A1 (en) * 2008-11-04 2010-05-14 Jean-Xavier Morin Method for the "co shift" conversion of a synthesis gas in a fast fluidised bed
CN101733045A (en) * 2008-11-14 2010-06-16 中国石油化工股份有限公司 Solid-liquid separation device and solid-liquid separation method for slurry bed reactor
CN101820991A (en) * 2007-08-24 2010-09-01 沙索技术有限公司 Process for producing liquid and gaseous products from gaseous reactants

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102190742B (en) * 2010-03-17 2013-02-06 中国石油化工股份有限公司 Olefin polymerization device and olefin polymerization method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3962070A (en) * 1972-01-03 1976-06-08 Hydrocarbon Research, Inc. H-coal process: slurry oil recycle system
US6822006B1 (en) * 2003-07-02 2004-11-23 Chevron U.S.A. Inc. Methods of controlling the temperature of an exothermic reaction
JP2006022283A (en) * 2004-07-09 2006-01-26 Nippon Steel Corp Slurry bed reaction system for bubbling tower type fisher-tropsh synthesis
CN101820991A (en) * 2007-08-24 2010-09-01 沙索技术有限公司 Process for producing liquid and gaseous products from gaseous reactants
WO2010052397A1 (en) * 2008-11-04 2010-05-14 Jean-Xavier Morin Method for the "co shift" conversion of a synthesis gas in a fast fluidised bed
CN101733045A (en) * 2008-11-14 2010-06-16 中国石油化工股份有限公司 Solid-liquid separation device and solid-liquid separation method for slurry bed reactor

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