WO2016180683A1 - Procédé et appareil pour la production de coke de pétrole calciné - Google Patents

Procédé et appareil pour la production de coke de pétrole calciné Download PDF

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Publication number
WO2016180683A1
WO2016180683A1 PCT/EP2016/059921 EP2016059921W WO2016180683A1 WO 2016180683 A1 WO2016180683 A1 WO 2016180683A1 EP 2016059921 W EP2016059921 W EP 2016059921W WO 2016180683 A1 WO2016180683 A1 WO 2016180683A1
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WO
WIPO (PCT)
Prior art keywords
reactor
petroleum coke
flue gas
process according
green
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2016/059921
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English (en)
Inventor
Edgar Gasafi
Peter Sturm
Günter Schneider
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Outotec Finland Oy
Original Assignee
Outotec Finland Oy
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Outotec Finland Oy filed Critical Outotec Finland Oy
Priority to US15/572,796 priority Critical patent/US20180112143A1/en
Priority to EP16720822.2A priority patent/EP3294846A1/fr
Priority to CN201680027118.0A priority patent/CN107636128B/zh
Publication of WO2016180683A1 publication Critical patent/WO2016180683A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L9/00—Treating solid fuels to improve their combustion
    • C10L9/08—Treating solid fuels to improve their combustion by heat treatments, e.g. calcining
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L5/00—Solid fuels
    • C10L5/02—Solid fuels such as briquettes consisting mainly of carbonaceous materials of mineral or non-mineral origin
    • C10L5/04—Raw material of mineral origin to be used; Pretreatment thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/02—Combustion or pyrolysis
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/06—Heat exchange, direct or indirect
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/10—Recycling of a stream within the process or apparatus to reuse elsewhere therein
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/14—Injection, e.g. in a reactor or a fuel stream during fuel production
    • C10L2290/143—Injection, e.g. in a reactor or a fuel stream during fuel production of fuel
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/14—Injection, e.g. in a reactor or a fuel stream during fuel production
    • C10L2290/145—Injection, e.g. in a reactor or a fuel stream during fuel production of air
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/58—Control or regulation of the fuel preparation of upgrading process

Definitions

  • the present invention relates to a process and an apparatus for the production of calcined green petroleum coke, wherein in a reactor green petroleum coke is combusted as a fuel with a substoichiometric amount of oxygen at a temperature of between 900 and 1400 °C to provide the required energy to evaporate volatile matter included in the green petroleum coke, wherein calcined petroleum coke and flue gas are obtained, and wherein the flue gas contains at least 80 wt-% of the volatile matter contained in the green petroleum coke.
  • Green petroleum coke (often abbreviated pet coke or petcoke) is a solid carbonization product from high-boiling hydrocarbon fractions obtained at temperatures below 630°C, e.g. in an oil refinery. Coking processes that can be employed for making petcoke include contact coking, fluid coking, flexicoking and delayed coking. Other coke has traditionally been delivered from coal.
  • This coke can either be fuel grade (high in sulfur and metals) or anode grade (low in sulfur and metals).
  • the raw coke directly out of the coker is often referred to as green coke.
  • green means unprocessed.
  • the petroleum coke is calcined to remove volatiles and then further processed at a temperature of at least 2500 °C to produce high-purity graphite petroleum coke, which is used e.g. for making anodes used in the steel and titanium smelter industry.
  • Green petroleum coke is mainly composed of elemental carbon (between 80 and 95 wt-%) in a polycrystallinet carbon matrix which is filled with volatile components such as hydrocarbons, sulfur-compounds and hydrogen.
  • the volatile content is generally between 9 and 21 wt % (see e.g. lUPAC (International Union of Pure and Applied Chemistry). 1995. Recommended Terminology for the Description of Carbon as a Solid. Pure Appl. Chem. 67(3):473-506.
  • the process and apparatus of the invention exclusively relate to the calcining step and do not refer to the subsequent production of high-purity graphite petro- leum coke.
  • the process of the invention comprises the combustion of green petroleum coke as a fuel inside of a reactor with a substoichiometric amount of oxygen at a temperature of between 900 and 1400 °C to provide the required energy to evaporate volatile matter included in the green petroleum coke.
  • calcined petroleum coke and flue gas are obtained, wherein the flue gas contains at least 80 wt-% of the volatile matter contained in the green petroleum coke.
  • the flue gas is at least partially recycled to the reactor as an additional fuel.
  • the process of the invention is superior to the prior art processes due to various reasons.
  • the volatile matter results in carbon monoxide (CO) and hydrogen (H 2 ) as major components.
  • the content depends largely on the composition of the feedstock and correspondents to the proximate analysis data.
  • the incineration of said compounds in the reactor protects the carbon in the petroleum coke from incineration/oxidation, since the volatile matter are easier combustible than the petroleum coke. Concluding, the recycled flue gas provides part of the energy necessary for calcining the petroleum coke, thereby increasing the carbon yield since less carbon of the green petroleum coke is burned.
  • Another advantage of the process according to the invention is the reduction of thermal strain on the calcining equipment due to the reduced temperature inside the reactor compared to prior art processes. This has multiple benefits: a re- Jerusalem temperature means reduced energy consumption for processing. It also allows to use lower grade refractory material inside the furnace, which reduces the capital investment for the plant.
  • the term "at least partially recycled” preferably refers to an amount of at least 10 vol-% of the flue gas being fed back into the reactor, more preferably to an amount of 20 -30 vol-% of the flue gas being fed back into the reactor.
  • the process of the invention employs a Lambda ( ⁇ -value) of less than 1 , preferably 0.25 -0.7.
  • the Lambda indicates the air-to-fuel ratio in the furnace. If lamb- da equals 1 , the air-fuel mixture is at the Stoichiometric ratio.
  • the process of the invention achieves a reduction of volatile matter to below 1 wt-% from a starting concentration of usually about 10 wt-% in untreated green petroleum coke. Due to the recycling of at least part of the flue gas and the reducing conditions in the reactor the process of the invention is superior to the state of the art both with regards to minimizing the loss of carbon from the green petroleum coke as well as the required amount of energy.
  • the green petroleum coke particles have a maximum diameter of 5 mm. Thereby, a complete calcining with a maximum carbon yield can be obtained.
  • the reactor is defined as a rotary kiln. This reactor type features the advantage of providing a continuous process with very good mass transfer. Further, the circulated gas stream is relatively small.
  • the reactor is defined as a fluidized bed reactor.
  • a fluidized bed reactor is characterized by a very good mass and heat transfer. The overall heat loss in a process according to the invention is very small. Even more preferred is an annular fluidized bed reactor.
  • the reactor temperature can be lowered to temperatures between 950 and 1200 °C due to the small heat loss. Thereby, the carbon yield can be increased even further since less fuel is required for providing the needed energy.
  • the recirculated flue gas is used as a fluidizing gas for the fluidizing gas reactor. So, the overall gas stream is kept constant in comparison to a conventional process. Further, the fuel can be introduced in the region of the reactor, namely into the fluidized bed, where the calcining of the green petrole- urn coke takes place and where the energy and therefore fuel burning is required.
  • the removed flue gas is fed into a Venturi pre-heater prior to recycling into the reactor for removal of solid particles.
  • Removed solid particles can be recycled to the reactor, too for increasing the carbon yield.
  • the Venturi is replaced by a filter.
  • the flue gas is fed from the Venturi pre-heater into a cyclone to achieve an additional purification and subsequently into at least one heat exchanger prior to recycling.
  • the energy of the flue gas can be used somewhere else in the process.
  • the flue gas Prior to recycling the flue gas from the at least one heat exchanger into the reactor, the flue gas may preferably be fed into a filter to remove any residual solid particles.
  • the oxygen source for the substoichiometric combustion pure oxygen, air or any other gas with at least 5 vol-% of oxygen is introduced in the reactor.
  • pure oxygen a very sensitive controlling of the introduced oxygen amount is possible.
  • the introduced gas stream is very small.
  • air is the cheapest oxygen source.
  • Using another gas stream with at least 5 vol-% of oxygen offers the possibility of using a gas stream incurred somewhere else in the process.
  • the gas stream which is introduced into the reactor in substoichiometric conditions is preheated, thereby reducing the energy requirements of the process of the invention even further.
  • the gas stream is preheated to a temperature of more than 400 °C.
  • the preheating is achieved by passing the gas stream through at least one heat exchanger. Even more preferably, said at least one heat exchanger is fed with the flue gas from the reactor.
  • the green petroleum coke can be fed directly into the reactor.
  • the green petroleum coke is preheated to a temperature of 400 °C in a heat exchanger before entering the reactor, preferably using at least part of the flue gas as a heat transfer medium.
  • This preheating is preferably effected in a Venturi pre-heater.
  • the preheated green petroleum coke is subsequently fed into a cyclone to concentrate the solid particles before guiding them into the reactor.
  • the Venturi pre-heater and a cyclone, used to preheat and concentrate the solid green petroleum coke particles are supplied with the flue gas from the reactor.
  • the recycled flue gas and air are fed separately into the reactor in order to avoid mixing and ignition prior to injection into the reactor.
  • the green petroleum coke is sufficiently calcined, it is preferably removed from the reactor and fed into a product cooler. When the cooling process is concluded, the calcined petroleum coke can be removed for further processing.
  • the present invention is also directed to an apparatus for the production of calcined petroleum coke.
  • Such an apparatus comprises a reactor for the com- bustion of green petroleum coke with a substoichiometric amount of oxygen at a temperature of between 900 and 1400 °C for obtaining calcined petroleum coke and flue gas.
  • This reactor features an inlet for feeding green petroleum coke into the reactor, an outlet for removing calcined petroleum coke from the reactor, a supply conduit for a gaseous oxygen source into the reactor and a gas outlet for the flue gas containing at least 80 wt-% of the volatile matter contained in the green petroleum coke.
  • a recycling conduit from the gas outlet into the reactor is foreseen to allow at least partial recycling of the flue gas.
  • a Venturi pre-heater is connected to the reactor. Even more prefera- bly, a cyclone and at least one heat exchanger are sequentially connected to the Venturi pre-heater.
  • the Venturi pre-heater has an inlet for feeding green petroleum coke into the pre-heater and an outlet for preheated green petroleum coke which is connected to the reactor. This advantageous embodiment reduces the energy that is required in the reactor to remove volatile components from the green petroleum coke.
  • the at least one heat exchanger has an inlet for air as well as outlets for flue gas and air which are connected to the reactor to enable recycled flue gas and air to be fed into the reactor.
  • the flue gas inlet into the reactor is located centrally to emulate an annular fluidized bed for ideal flue gas incineration conditions.
  • the reactor is preferably equipped with an outlet for the removal of calcined green petroleum coke. Said outlet is preferably connected to a product cooler where the sufficiently cooled final product is removed for further processing.
  • the recycling of the flue gas can be effected by various means which are known to the skilled person. For instance, a gas compressor may be used to transport the flue gas from the heat exchanger(s) back into the reactor.
  • the flue gas is de-dusted prior to compression. De-dusting can be effected by e.g. a filter or a Venturi.
  • the flue gas may be transported from the heat exchanger(s) to the reactor by employing a thermo compressor with steam injection.
  • FIG 1 shows schematically the process according to the invention.
  • the green petroleum coke with a solid matter content of about 90 wt-% carbon and 10 wt-% volatiles is calcined at a temperature of 1 100 °C for 30 min in a fluidized bed reactor 10 before being removed via outlet conduit 1 1 into cooler 12 before being discharged through conduit 13.
  • the produced flue gas is continuously removed from the reactor through an outlet and fed via outlet conduit 14 into a Venturi pre-heater 20 together with fresh green petroleum coke fed from conduit 21 .
  • This enables the fresh green petroleum coke to be preheated to a temperature of between 350 and 500 °C, reducing the required energy for calcining the green petroleum coke in the reactor 10.
  • the green petroleum coke particles have a diameter of less than 5 mm.
  • the flue gas/green petroleum coke mixture is subsequently moved through conduit 22 into cyclone 23 to separate the solid material from the flue gas.
  • the solid material is fed via conduit 24 and inlet conduit 25 into the fluidized bed reactor 10, while the flue gas is directed through conduit 26 into a first heat exchanger 30 and subsequently through conduit 31 into a second heat exchanger 32.
  • the flue gas is used as a heat transfer medium to heat a gas stream.
  • the flue gas is directed via conduit 33 through a filter 34 to remove any residual solid particles. Solid particles can be recycled via conduit 38 into the inlet conduit 25 for the solid inlet or directly into the reactor 10.
  • Part of the flue gas (10 - 30 %) is branched off from conduit 35 coming out of the filter 34 and is recycled via recycling conduits 40 and 41 into reactor 10. By passing the heat exchanger 30, it is further heated up again to 500 °C. The remaining amount of flue gas removed from the process via conduit 36. Air is fed into the second heat exchanger 32 via conduit 42 and heated to a temperature of about 400 °C.
  • the flue gas and the air are separately injected into the reactor 10 through recycling conduit 41 and supply conduit 43 to avoid premature mixing and igni- tion.
  • the ratio by weight of air and recycled flue gas is between 0,3 to 0,6 preferably 0.4 - 0,5.
  • the flue gas and air are fed into the reactor 1 through a central nozzle 50 for optimal incineration conditions.
  • a typical composition of the flue gas upon entering the reactor 1 is for example:
  • This process results in a calcined petroleum coke having a residual content of volatiles of less than 1 wt-%.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Coke Industry (AREA)

Abstract

La présente invention concerne un procédé de production de coke de pétrole calciné. Dans un réacteur de coke de pétrole vert est brûlée en tant que combustible une quantité sub-stœchiométrique d'oxygène à une température comprise entre 900 et 1400 °C pour fournir l'énergie requise pour évaporer une matière volatile incluse dans le coke de pétrole vert. Du coke de pétrole calciné et du gaz de combustion sont obtenus, le gaz de combustion comprenant au moins 80 % en poids de la matière volatile contenue dans le coke de pétrole vert. Le gaz de combustion est au moins partiellement recyclé vers le réacteur en tant que combustible additionnel.
PCT/EP2016/059921 2015-05-12 2016-05-03 Procédé et appareil pour la production de coke de pétrole calciné Ceased WO2016180683A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US15/572,796 US20180112143A1 (en) 2015-05-12 2016-05-03 Process and apparatus for the production of calcined petroleum coke
EP16720822.2A EP3294846A1 (fr) 2015-05-12 2016-05-03 Procédé et appareil pour la production de coke de pétrole calciné
CN201680027118.0A CN107636128B (zh) 2015-05-12 2016-05-03 用于生产经煅烧的石油焦炭的方法和装置

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015107433.8 2015-05-12
DE102015107433.8A DE102015107433A1 (de) 2015-05-12 2015-05-12 Verfahren und Anlage zur Produktion von kalziniertem Petrolkoks

Publications (1)

Publication Number Publication Date
WO2016180683A1 true WO2016180683A1 (fr) 2016-11-17

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ID=55913624

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Application Number Title Priority Date Filing Date
PCT/EP2016/059921 Ceased WO2016180683A1 (fr) 2015-05-12 2016-05-03 Procédé et appareil pour la production de coke de pétrole calciné

Country Status (5)

Country Link
US (1) US20180112143A1 (fr)
EP (1) EP3294846A1 (fr)
CN (1) CN107636128B (fr)
DE (1) DE102015107433A1 (fr)
WO (1) WO2016180683A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN119736102B (zh) * 2024-12-25 2025-10-31 山东大学 一种石油焦的资源化利用方法和系统

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US3271268A (en) * 1963-01-21 1966-09-06 Marathon Oil Co Process of calcining coke
US4022569A (en) * 1975-12-05 1977-05-10 Alcan Research And Development Limited Calcination of coke
US4407700A (en) * 1982-06-14 1983-10-04 Conoco Inc. Injector for calciner
WO2005014866A2 (fr) * 2003-08-09 2005-02-17 Outokumpu Technology Oy Procede et installation pour la reduction de matieres solides contenant de l'oxyde de fer

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US3271268A (en) * 1963-01-21 1966-09-06 Marathon Oil Co Process of calcining coke
US4022569A (en) * 1975-12-05 1977-05-10 Alcan Research And Development Limited Calcination of coke
US4407700A (en) * 1982-06-14 1983-10-04 Conoco Inc. Injector for calciner
WO2005014866A2 (fr) * 2003-08-09 2005-02-17 Outokumpu Technology Oy Procede et installation pour la reduction de matieres solides contenant de l'oxyde de fer

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Title
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PREDEL: "Ullmann's Encyclopedia of Industrial Chemistry", 2006, article "Petroleum Coke"

Also Published As

Publication number Publication date
EP3294846A1 (fr) 2018-03-21
CN107636128A (zh) 2018-01-26
CN107636128B (zh) 2021-04-20
DE102015107433A1 (de) 2016-11-17
US20180112143A1 (en) 2018-04-26

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