US3887453A - Process for obtaining oil, gas and byproducts from pyrobituminous shale or other solid materials impregnated with hydrocarbons - Google Patents

Process for obtaining oil, gas and byproducts from pyrobituminous shale or other solid materials impregnated with hydrocarbons Download PDF

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Publication number
US3887453A
US3887453A US285692A US28569272A US3887453A US 3887453 A US3887453 A US 3887453A US 285692 A US285692 A US 285692A US 28569272 A US28569272 A US 28569272A US 3887453 A US3887453 A US 3887453A
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retort
retorting
shale
gases
solid materials
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Seiki Ueta
Osmar Chaves Ivo
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Petroleo Brasileiro SA Petrobras
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Petroleo Brasileiro SA Petrobras
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    • 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
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/02—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by distillation

Definitions

  • FIG. 3 UNITED STATES PATENTS 3,228,869 1/1966 Irish 208/11 8 Claims, 4 Drawing Figures see-M53 SHEET 3 2?) FIG. 3
  • An object of this invention is to provide the operating system with means for substantially increasing the extraction of mineral oil and other derivatives from shale.
  • a technique is employed such that a mist is formed by the carrier recycling gases for carrying with it the largest possible amount of extracted material.
  • a further object of this invention is to make the process cheaper, due to the specific carrier recycling gas conditions which increase the output.
  • the system consists of a vertical cylindrical retort, with tapered ends through the upper end of which the shale is fed in pieces for downward flow thereof in moving countercurrent with the heated gases. Thereafter the shale is discharged through the bottom of reactor.
  • the recycling gases, heated outside the retort, are introduced through the bottom of the reactor, moving in countercurrent with the descending shale, and leave the retort by a side pipe at the top thereof in the form of a mist saturated with extracted material and carrying the partially condensed pyrolysis products
  • the dif ferent systems vary in the basic operation, modes of heating, heating mediums, heat sources, positions of the heat sources, shale aggregation state, frequency of operation, direction of heating, moving of shale in pyrolysis and, finally, the pyrolysis gas dilution.
  • Each of these variation conditions gives rise to other such deviations, which may be combined in a plurality of systems defining the type employed.
  • Another important point is that the recycling gases coming from the retort in the form of a mist pass through a filtration, separation and condensation system before being heated. Equally important is the introduction of recycling the extraction gases at such a temperature and rate that a mist is permitted to form, this being important for the good performance of the process.
  • the recycled extraction gas will pass through the bed in upwardly, in countcrcurrent with the shale, at a rate not less than 0.2 to 2.0 meters per second.
  • the mist formed should leave with 5% minimum and 25% maximum of condensed material with respect to the pyrolysis products, and at a temperature ranging from 121C to 177C.
  • FIG. I shows diagrammatically a system according to the invention
  • FIG. 2 shows one embodiment of the hopper and rotating valve 3 arrangement of FIG. 1;
  • FIG. 3 shows a second embodiment of the hopper and valve (3) arrangement of FIG. 1;
  • FIG. 4 is a graph showing various retort bed temperature profiles.
  • the process consists of a system in which the shale, which is mined in pieces of usually not less than a minimum 3.6mm (Vs in) to 200mm (8 inches) and, if desired, mixed with briquettes made of fines produced in the crushing, is carried to a retort by a conveyor belt 1 or other suitable elevator means; from there it passes into a hopper 2 and then through a rotary valve 3 dynamically sealed by an inert gas; next it is passed to an elongated vertical vessel, preferably of circular section, provided with a device for controlling the solids level alarm which controls the speed of conveyor belt 1.
  • This device employs gamma rays or other suitable means.
  • the retort consists of a vertical cylindrical vessel whose wall is provided with an internal lining of refractory material 7 covered by a protective metallic coating and an outer layer of thermal insulating material. In its downward vertical movement the shale passes in succession through preheating, drying and retort zones located in the space between the top of the bed and the hot gas distributors 8 where due to the high temperatures, successively its moisture and volatile products, usually gaseous and liquids are liberated.
  • the gaseous fraction consisting of inorganic and organic gases in variable ratios depending on the nature of the material and the retort conditions, normally contains hydrocarbons, hydrogen and hydrogen sulphide gas as main constituents.
  • the liquid fraction consists of the moisture set free in drying and retorting, and of oil, this latter being of complex composition and hereinafter to be called "shale oil.
  • a non-volatile organic residue, hereinafter referred to as coke will remain in the solids.
  • exhaust shale The solids and coke, from now on referred to as exhaust shale, pass through the cooling zone 9 located between the hot gas distributors 8 and a discharge mechanism comprising deflectors 10, fixed retarding plates 11 and a speed controlled movable grid 12 which makes a translational movement around the retort axis.
  • this mechanism-especially developed for providing a continuous uniform flow of the mined shale subject to the action of gravity in large diameter cylindrical vessels the shale rests on the deflector assembly l0 and retarding or resting plates 11 in virtue of its angle of repose, there being no flow when the movable grid 12 is at the rest (the whole discharge or outlet system is described in Brazilian Pat. No. 69.423 granted on Apr. 29, 1964).
  • the shale is forced to move horizontally and alternately towards the internal and external circumferences of retarding plates 11, from where it freely falls into a hop per 13 which forms the conical retort bottom passing through a cold gas distributor 14.
  • a speed controlled rotary valve 15 from the level controller to a tank 16 that has the double function of providing hydraulic sealing for said rotary valve and means for making a sludge of the retorted shale and water.
  • the rotary valve is also dynamically sealed by inert gas, then dispensing with the water seal; second, two series connected valves are used, the sealing gas entering the interconnecting conduit.
  • Cold gas is admitted to the retort through the gas distributor 14, consisting of several horizontal tubes paral lelly disposed with respect to each other and provided of two rows of holes spaced at about 90 to each other; each rows of holes delivers several gas jets downwardly at an angle of about 45 to the vertical, thus providing homogeneous distribution of gas in the whole reactor bottom section and preventing entrance of shale into the holes and the actual distributor pipes.
  • the gas distributor 14 consisting of several horizontal tubes paral lelly disposed with respect to each other and provided of two rows of holes spaced at about 90 to each other; each rows of holes delivers several gas jets downwardly at an angle of about 45 to the vertical, thus providing homogeneous distribution of gas in the whole reactor bottom section and preventing entrance of shale into the holes and the actual distributor pipes.
  • the cold gas gage pressure at the retort input is 0.3 to 1.5 atmospheres, which is sufficient to overcome the combined resistence of the bed of solids, the circulation conduits and devices, while still maintaining the whole system at a pressure slightly above atmospheric, this preventing leakage of air into the apparatus, and its temperature is superior to the room temperature although substantially less than the destructive distillation temperature named in this specification retorting temperature," which is usually about lOOC.
  • the cold gas In its upward path the cold gas exchanges sensible heat with the hot descending solid the exhaust shale that gives up the major part of its heat and leaves the retort at a temperature substantially lesser than the retorting temperature, i.e., at the cold exhaust shale temperature, usually of from 200C to 300C.
  • the cold gas reaching the retorting zone at a temperature similar to but less than the retorting temperature is mixed with the hot gas admitted through the respective distributor.
  • This hot gas distributor 8, formed similarly to the cold gas distributor 14, consists ofa metal suitable for resisting high temperatures and is provided with deflectors coupled to the tubes positioned above them.
  • Said deflectors are designed to protect the pipes from the abrasion caused by the solids and deviate the flow of solids to the free spaces existing between the distributor tubes and between the tubes and the internal wall of retort.
  • the gas entering the retort through the hot gas distribu tor 8 enters at a temperature above the retorting temperature and under a pressure slightly less than the inlet pressure of the cold gas, these pressures differing as a function of the mechanical resistence to which the gas is subjected in its upward path; said hot gas inlet temperature usually ranges from 400C to 800C.
  • the gas passing through the exhaust shale refrigerating zone 9 is mixed with the hot gas, the ratio of hot gas to cold gas being regulated in such a way that the resulting temperature is the retorting temperature; the resulting amount of gas is regulated so that during its upward flow it gives off sufficient sensible heat to effect successively and from the bottom to the top, the retorting, heating and drying of the shale.
  • the shale is at the same time heated in the retorting zone and sets free generally gaseous or normally liquid compounds, of organic and inorganic nature, which are produced by thermal decomposition of the organic matter spread through the mineral mass, and by the thermal decomposition of some inorganic compounds also present.
  • main compounds usually contained in the retorted product are hydrogen sulphide gas, carbon dioxide, hydrogen, saturated and normally gaseous insaturated aliphatic hydrocarbons, and organic compounds normally liquids called shale oil that consist of aliphatic saturated and insaturated, naphtenic and aromatic hydrocarbons and of heterocyclic organic compounds containing oxigen, nitrogen or sulfur, and of the water formed in the thermal decomposition of the organic and inorganic compounds.
  • the gases give up sensible and latent heat in order simultaneously to heat the solids, evaporate moisture from the shale and to cool themselves to a temperature ranging from [00C to 150C, at which most of the normally liquid fractions are condensed to a fine heavy oil mist from the shale that is drawn by the mixture of heat carrier gases with the gases produced by retorting.
  • the gases and mist of heavy shale oil pass into a chamber 6, solid free, where its ascending speed is from 0.5 to 2.0 meters per second, and where only a dust of shale and the mist of oil are drawn.
  • the gases are led through the vertical collecting tubes 18 positioned at the top pf the retort in such a way as to maintain an homogeneous upward gas speed to one or more convergent conduit systems 19, of increasing sectional areas, designed in such a way that the speed of the gases entering the collecting tubes 18 remains approximately constant;
  • the large cross section end segments are connected through tubes 19 with the inlet of one or more centrifugal separators, preferably cyclones 20 in series with electrostatic precipitators 22, through tube 21 where the gases are freed of mist and dust.
  • Such separators are designed to retain in the coarser particles of solids and oil in the cyclone 20 and the finer particles in the electrostatic precipitators 22.
  • the system efficiency is from to 99.9%.
  • the cyclones 20 have inlets 23 for the shale oil in order to facilitate the continuous or intermittent washing of its walls, in order to avoid deposition of dust and heavy oil; and from there the liquid and solid materials leave through tubes 24 to a separating apparatus 25 from which the liquid is passed through tubes 26 and 32 to settlers 33 and the solids to the waste, through conduits 27 and 35; the liquid may contain some condensed water, as a consequence of the slight cooling due to the heat loss of the gases through the walls of the apparatus.
  • the electrostatic precipitators 22 which may also be oil washed admitted through the tubes 28, as in the case of cyclones, the finer particles are separated from the oil, dust and condensed liquids; all the solid and liquid materials are drained through the tubes 29 and separating apparatus 30 ensures that the liquids 6 are passed through the tubes 31 and 32 to the settlers e 33 and the solids to the waste, through the tubes 34 and 15; 9012, 35.
  • the OII fractions separated in the settlers 33 are G asflossgs f 2.41 2.09 ar on( ry asis).
  • d I113 985 passed through the tubes 36 pump 37 and tubes 38 to Hydrogen (dry basis) q 2) L56 storage, and the water fractions, through the tubes 39, 5 Sulfur (dry basis).
  • the gas admitted to the bottom section of cooler 43 is cooled by direct contact in countercurrent with a TABLE I" water spray 61 or cold light oil spray that falls from the top of the vessel and leaves through pipe 50 for further r g treatment.
  • the condensed products in the cooler are LRTIES OF SHALE drained along with water or oil admitted in the top via Components Volume '12 pipe 51 to the settler 52 where the light oil and water H2O 1.28 are separated.
  • the 01] is passed to storage through the 15 pipe 53 while the water is passed through the pipe 54 (:rHm 1.41 to pump 55 and thereafter to the waste or treatment, through pipes 56 and 57 and to recycle in the cooler I3 43, through pipe 58, exchanger 59 and pipe 60.
  • Table I shows H28 25.8l the result of laboratory tests of two average Samples, 3%? RSH representing the feed used in the retorting operation; in C0 L67 Table II and III are the results of laboratory tests of oil 8 and gas obtained in several tests of the retorting opera- 5 tions; Table IV shows the tests of exhaust shale produced in various retorting operations; and Table V is an abstract of operational conditions of some retorting op erations and respective yields.
  • a non-combustion process for obtaining mineral oil and other derivatives from pyrobituminous shale or other solid materials impregnated with hydrocarbons the said process being non-combustive and carried out in a vertical distillation retort, wherein the mined shale or other solid materials is continuously fed at the top of said retort through an inert gas sealed valve, wherefrom said mined shale or other solid materials are evenly distributed to the retorting zone and then descend to a cooling zone below the retorting zone.
  • the retorting being carried out at super-atmospheric pressure by a mixture of substantially oxygen-free recycling gases previously and indirectly heated outside the retort.
  • said heated recycling gases being introduced into the bottom of the retorting zone of said retort at a higher temperature than the retorting temperature, and of substantially oxygen-free recycling gases introduced cold at the bottom of said retort into the cooling zone which in upwardly flow through the cooling zone exchange sensible heat with said retorted shale or other solid materials that is continuously withdrawn from the bottom of said retort through an inert gas sealed valve.
  • the liquid and gaseous retorting products being drawn from top of said retort.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
US285692A 1971-09-06 1972-09-01 Process for obtaining oil, gas and byproducts from pyrobituminous shale or other solid materials impregnated with hydrocarbons Expired - Lifetime US3887453A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
BR5857/71A BR7105857D0 (pt) 1971-09-06 1971-09-06 Processo aprefeicoado para obtencao de oleo gas e subprodutos de xisto pirobetuminosos ou outros materiais impregnados com hidrocarbonetos

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US (1) US3887453A (de)
AR (1) AR198631A1 (de)
AU (1) AU473288B2 (de)
BR (1) BR7105857D0 (de)
DE (1) DE2243389B2 (de)
ES (1) ES406426A1 (de)
FR (1) FR2152616B1 (de)
GB (1) GB1396018A (de)
IE (1) IE36666B1 (de)
SE (1) SE405125B (de)
ZA (1) ZA726079B (de)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4088562A (en) * 1975-11-19 1978-05-09 Twenty Farms, Inc. Method and apparatus for processing oil shale
US4116810A (en) * 1976-05-24 1978-09-26 Paraho Corporation Indirect heating pyrolysis of oil shale
US4388173A (en) * 1980-06-25 1983-06-14 Veba Oel Ag Method and apparatus for distillation of oil shale
US4536279A (en) * 1984-01-19 1985-08-20 Mobil Oil Corporation Enhanced recovery of hydrocarbonaceous fluids from oil shale
GB2199043A (en) * 1986-12-22 1988-06-29 Petroleo Brasileiro Sa Apparatus and process for obtaining oil, gas and by-products from pyrobituminous shale and other material impregnated with hydrocarbons
US5041210A (en) * 1989-06-30 1991-08-20 Marathon Oil Company Oil shale retorting with steam and produced gas
US5068010A (en) * 1986-12-22 1991-11-26 Petroleo Brasileiro S.A. - Petrobras Apparatus for securing oil, gas and by-products from pyrobituminous shale and other matter impregnated with hydrocarbons
US20080135457A1 (en) * 2006-12-11 2008-06-12 Ridge Raymond L Method and apparatus for recovering oil from oil shale without environmental impacts
CN102161900A (zh) * 2011-03-21 2011-08-24 唐山雷浩能源技术装备有限公司 一种高效块状油页岩提油的装置及方法
CN102161899A (zh) * 2011-03-21 2011-08-24 唐山雷浩能源技术装备有限公司 一种高效内热式粉末油页岩提油装置及其方法
US8894939B2 (en) * 2010-08-16 2014-11-25 Emerging Fuels Technology, Inc. Three phase reactor
CN104498069A (zh) * 2014-12-30 2015-04-08 汪清县龙腾能源开发有限公司 一种干排焦气体热载体油页岩干馏工艺
US9795972B2 (en) 2012-08-07 2017-10-24 Cameron International Corporation High temperature high pressure electrostatic treater

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002064702A1 (de) 2001-02-09 2002-08-22 Stierli + Ruggli Bindemittel und verfahren zur herstellung eines bindemittels für bodenstabilisierungen, sowie böden, wände oder trennschichten, welche unter verwendung eines solchen bindemittels oder verfahrens stabilisiert wurden
US9457337B2 (en) * 2013-03-01 2016-10-04 Praxair Technology, Inc. Adsorbent composition for argon purification
WO2015053721A1 (en) * 2013-10-11 2015-04-16 Al Ahmad Trad High range temperature thermal dismantling method in processing oil shale
CN106635082A (zh) * 2017-02-24 2017-05-10 山东腾鲁环保设备有限公司 一种高温干馏系统

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3228869A (en) * 1964-05-19 1966-01-11 Union Oil Co Oil shale retorting with shale oil recycle
US3384569A (en) * 1966-02-21 1968-05-21 Exxon Research Engineering Co Oil shale retorting
US3484364A (en) * 1967-03-02 1969-12-16 Exxon Research Engineering Co Fluidized retorting of oil shale
US3503869A (en) * 1967-02-23 1970-03-31 Mobil Oil Corp Process for improving thermal efficiency of gas combustion shale retorting
US3526586A (en) * 1966-10-21 1970-09-01 Arthur L Saxton Retorting of oil shale
US3551322A (en) * 1967-04-03 1970-12-29 Phillips Petroleum Co Conversion of oil shale retorting gases
US3619405A (en) * 1968-07-10 1971-11-09 Continental Oil Co Gas combustion oil shale retorting with external indirect gas heat exchange

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3228869A (en) * 1964-05-19 1966-01-11 Union Oil Co Oil shale retorting with shale oil recycle
US3384569A (en) * 1966-02-21 1968-05-21 Exxon Research Engineering Co Oil shale retorting
US3526586A (en) * 1966-10-21 1970-09-01 Arthur L Saxton Retorting of oil shale
US3503869A (en) * 1967-02-23 1970-03-31 Mobil Oil Corp Process for improving thermal efficiency of gas combustion shale retorting
US3484364A (en) * 1967-03-02 1969-12-16 Exxon Research Engineering Co Fluidized retorting of oil shale
US3551322A (en) * 1967-04-03 1970-12-29 Phillips Petroleum Co Conversion of oil shale retorting gases
US3619405A (en) * 1968-07-10 1971-11-09 Continental Oil Co Gas combustion oil shale retorting with external indirect gas heat exchange

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4088562A (en) * 1975-11-19 1978-05-09 Twenty Farms, Inc. Method and apparatus for processing oil shale
US4116810A (en) * 1976-05-24 1978-09-26 Paraho Corporation Indirect heating pyrolysis of oil shale
US4388173A (en) * 1980-06-25 1983-06-14 Veba Oel Ag Method and apparatus for distillation of oil shale
US4536279A (en) * 1984-01-19 1985-08-20 Mobil Oil Corporation Enhanced recovery of hydrocarbonaceous fluids from oil shale
GB2199043B (en) * 1986-12-22 1991-09-11 Petroleo Brasileiro Sa Apparatus and process for obtaining oil, gas and by-products from pyrobituminous shale and other material impregnated with hydrocarbons
US4944867A (en) * 1986-12-22 1990-07-31 Petreleo Brasileiro S.A. - Petrobras Process to secure oil, gas, and by-products from pyrobetuminous shale and other matter impregnated with hydrocarbons
AU608555B2 (en) * 1986-12-22 1991-04-11 Petroleo Brasileiro S.A. - Petrobras Improvement to equipment and process to secure oil, gas, and by-products from pyrobituminous shale and other matter impregnated with hydrocarbons
GB2199043A (en) * 1986-12-22 1988-06-29 Petroleo Brasileiro Sa Apparatus and process for obtaining oil, gas and by-products from pyrobituminous shale and other material impregnated with hydrocarbons
US5068010A (en) * 1986-12-22 1991-11-26 Petroleo Brasileiro S.A. - Petrobras Apparatus for securing oil, gas and by-products from pyrobituminous shale and other matter impregnated with hydrocarbons
US5041210A (en) * 1989-06-30 1991-08-20 Marathon Oil Company Oil shale retorting with steam and produced gas
US7807049B2 (en) 2006-12-11 2010-10-05 Ridge Raymond L Method and apparatus for recovering oil from oil shale without environmental impacts
US20080135457A1 (en) * 2006-12-11 2008-06-12 Ridge Raymond L Method and apparatus for recovering oil from oil shale without environmental impacts
US8894939B2 (en) * 2010-08-16 2014-11-25 Emerging Fuels Technology, Inc. Three phase reactor
CN102161900A (zh) * 2011-03-21 2011-08-24 唐山雷浩能源技术装备有限公司 一种高效块状油页岩提油的装置及方法
CN102161899A (zh) * 2011-03-21 2011-08-24 唐山雷浩能源技术装备有限公司 一种高效内热式粉末油页岩提油装置及其方法
CN102161899B (zh) * 2011-03-21 2013-05-08 唐山雷浩能源技术装备有限公司 一种高效内热式粉末油页岩提油装置及其方法
CN102161900B (zh) * 2011-03-21 2014-05-28 唐山雷浩能源技术装备有限公司 一种高效块状油页岩提油的装置及方法
US9795972B2 (en) 2012-08-07 2017-10-24 Cameron International Corporation High temperature high pressure electrostatic treater
CN104498069A (zh) * 2014-12-30 2015-04-08 汪清县龙腾能源开发有限公司 一种干排焦气体热载体油页岩干馏工艺

Also Published As

Publication number Publication date
ZA726079B (en) 1973-06-27
AU473288B2 (en) 1976-06-17
FR2152616A1 (de) 1973-04-27
BR7105857D0 (pt) 1973-04-10
DE2243389A1 (de) 1973-03-15
DE2243389B2 (de) 1976-04-22
IE36666L (en) 1973-03-06
IE36666B1 (en) 1977-01-19
FR2152616B1 (de) 1978-12-22
GB1396018A (en) 1975-05-29
SE405125B (sv) 1978-11-20
ES406426A1 (es) 1975-07-16
AR198631A1 (es) 1974-07-15
AU4579372A (en) 1974-02-28

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