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WO2000044854A1 - Distillation discontinue thermolytique de matiere carbonee - Google Patents

Distillation discontinue thermolytique de matiere carbonee Download PDF

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Publication number
WO2000044854A1
WO2000044854A1 PCT/US1999/030002 US9930002W WO0044854A1 WO 2000044854 A1 WO2000044854 A1 WO 2000044854A1 US 9930002 W US9930002 W US 9930002W WO 0044854 A1 WO0044854 A1 WO 0044854A1
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
lid
molten material
process according
basket
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/US1999/030002
Other languages
English (en)
Inventor
William Dell'orfano
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.)
Sector Capital Corp
Original Assignee
Sector Capital Corp
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 Sector Capital Corp filed Critical Sector Capital Corp
Publication of WO2000044854A1 publication Critical patent/WO2000044854A1/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
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B49/00—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated
    • C10B49/14—Destructive distillation of solid carbonaceous materials by direct heating with heat-carrying agents including the partial combustion of the solid material to be treated with hot liquids, e.g. molten metals
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the invention relates generally to transformation of carbonaceous material such as waste wood into liquid hydrocarbons and char.
  • a principal object of the present invention is to provide an improved process and distillation unit for on- site thermal conversion of scrap wood or other organic matter into commercially desirable products in a way that minimizes the disposal problems faced by the owners of sites that create significant quantities of scrap wood. Further objects are to provide an improved process and distillation unit wherein scrap wood is immersed in molten material and thereby converted to gaseous hydrocarbons and char; to further provide such a process wherein scrap wood is thermally converted to vapor forms that may be condensed and further separated to commercially valuable hydrocarbons and char; to further provide such a process wherein residual solids from the thermal conversion, including char, are captured and separated; to further provide such a process wherein a portion of the combustible vapors emitted from the thermal conversion of organic matter is utilized to heat the molten material bath in the reaction bath; to further provide such a process and apparatus that minimizes the risk of exposure of operating personnel to the high temperatures of the molten material; to further provide such a process wherein the self-ignition
  • the present invention provides an apparatus and process for batch thermolytic distillation of lump carbonaceous material .
  • a preferred embodiment of the apparatus includes a distillation unit including a reactor with a reactor bath adapted to hold a molten material selected from a group of molten materials consisting of molten metal and molten salt, a retractable lid, and a basket pivotally mounted within the reactor bath between a pair of opposing reactor bath walls.
  • the reactor In a distillation unit intended for side-by-side mounting of multiple units and for receiving a charge of wood from above a first end of the unit, the reactor is located at a first end of the unit, and the basket is pivotally mounted for rotation toward a second end of the unit, opposite the first end.
  • the preferred embodiment includes at least one hydraulic hold-down clamp attached between reactor and lid.
  • the lid includes a perimeter curtain wall having a beveled lower rim shaped to fit a facing beveled rim of the reactor bath, and a perforated screen.
  • the reactor further includes an inlet conduit for molten material, an outlet conduit for molten material, and a reactor gas outlet; and the unit further includes a reservoir for storing molten material, the reservoir having a supply conduit coupled to supply molten material to the reactor inlet conduit, and a return conduit coupled to accept molten material from the reactor outlet conduit.
  • the base of the reactor is higher than the top of the reservoir by approximately three feet .
  • the reservoir includes two compartments with a check valve connecting them, a pressurized air inlet, and a controllable vent.
  • the reservoir also includes an excess-air heater, and a corrugated heat exchanger.
  • the distillation unit further comprises a steam generator with a flu pipe and the reservoir further includes an excess-air heater flu, and a bypass flu pipe with a control valve .
  • the bypass flu pipe is connected between the excess-air heater flu and the steam generator flu pipe.
  • the reactor bath includes a wall conduit.
  • the distillation unit further includes a condenser with a particulates trap having a pressure region below atmospheric pressure .
  • the present invention also provides a process for batch thermolytic distillation of carbonaceous material .
  • the process includes rotating a porous basket into a reactor bath; putting a charge of wood into the basket; closing a retractable lid onto the reactor bath; and filling the reactor bath with molten material to produce gas and char by thermolytic conversion of the charge .
  • the molten material is preferably molten tin at a temperature of approximately 455°C.
  • Rotating the porous basket into the reactor bath includes rotating the basket about an axis within the reactor bath.
  • Closing the lid includes translating the lid and lowering the lid.
  • the preferred embodiment further includes forcibly holding the lid closed while the temperature in the reactor bath is above a predetermined temperature .
  • Filling the reactor with molten material includes moving molten material by gravity or by air pressure .
  • the process preferably includes moving molten material through the basket for a predetermined period of time after filling the reactor bath with molten material, and raising the surface of the molten material at a sufficient rate to ensure that steam given off from newly heated charge effectively prevents oxygen from reacting with newly formed char.
  • the molten material is preferably heated using an excess air heater using combustible fluids produced in the reactor bath and further using heat from hot air recovered during condensing to heat the molten material .
  • a flow of molten material through the reactor bath is preferably maintained during thermolytic distillation.
  • the process further includes draining the reactor bath of molten material while the lid is closed; quenching the char in the reactor bath with steam; opening the lid; and removing the char from the basket .
  • Draining the reactor bath includes driving superheated steam into the reactor bath. Superheated steam is produced at a temperature of about 228°F, and a pressure of about 20psi, using flu gas from an excess air heater. The char is quenched with steam until the temperature of the char is below a self-ignition temperature. Opening the lid includes raising the lid using hydraulic actuators, and retracting the lid using a drive screw to place the lid under a lip of a loading platform. Removing the char from the basket includes rotating the basket about an axis within the reactor bath.
  • the process further includes condensing, in a pressure region below atmospheric pressure, a mixture of gas from thermolytic conversion of the charge and steam introduced in quenching.
  • FIG. 1 is a schematic representation of a first embodiment of the distillation unit of the invention.
  • FIG. 2 is a partial cut-away perspective view of multiple distillation units of FIG.l between an on-site loading platform and a belt conveyor system.
  • FIG. 3A is a cut-away elevation view of the reactor, the loading platform, and the reactor lid of FIG 1, illustrating the retraction and replacement of the lid.
  • FIG. 3B is a perspective view of the lid carrier and basket carrier of the embodiment of FIG.l.
  • FIG. 3C is a schematic elevation view of the lid carrier and basket carrier of FIG. 3B, giving more detail.
  • FIG. 3D is a cut-away perspective view of the basket carrier and pivot plate of the embodiment of FIG. 1.
  • FIG. 4 is a schematic elevation view of the reactor, the loading platform, and the basket of FIG.l, illustrating the loading of the basket with wood.
  • FIG. 5 is a schematic elevation view of a portion of FIG.l, showing the basket tipping the char onto the conveyor system.
  • FIG. 6 is a schematic perspective view of a portion of the embodiment of FIG.l, illustrating the flow of molten metal through the reservoir and through the reactor.
  • FIG. 7A is a schematic perspective view of a portion of the reservoir, showing the excess-air heater.
  • FIG. 7B is an enlarged portion of FIG. 7A, giving detail of the excess-air heater.
  • FIG. 8 is a schematic perspective view of the condenser of FIG.l.
  • the invention provides a process and a distillation unit for converting carbonaceous material into useful product by thermolysis (dissociation of a compound by heat in a bath of molten metal, or molten salt, in the absence of oxygen) .
  • the invention provides a process for converting wood to wood- petrol and char by immersion in molten tin at a temperature of approximately 851°F (455°C) .
  • the Distillation Unit Distillation unit 11 of the preferred embodiment, which includes frame 10, is shown in FIG. 1 between loading platform 110 and belt conveyor system 120.
  • FIG. 1 shows reactor bath 19 of reactor 20 in the reaction phase containing molten tin 21 and porous basket 30, with retractable lid 40 on top of the reactor.
  • the front of distillation unit 11 is shown beneath loading platform
  • FIG. 2 Multiple distillation units, 11, 12, 13, etc. may be mounted side-by-side, as shown in FIG. 2, to match the throughput requirements of a given site.
  • the retraction and replacement of the lid with respect to loading platform 110 and conveyor system 120 is shown in FIG. 3A.
  • the loading of reactor 20 with a charge of lump wood 100 from the loading platform is shown in FIG.
  • FIG. 1 shows reactor 20 having a reactor gas outlet 25, an inlet conduit 26, and an outlet conduit 27.
  • basket 30 The purpose of basket 30 is to contain wood in the reactor before and during the reaction phase and to carry char out of the reactor after the reaction phase.
  • the walls of the basket are made of heavy wire mesh or heavy pressed steel having multiple apertures 38 which allow the molten tin to penetrate the basket and contact the lump wood.
  • the basket is 60 inches long, 36 inches deep and 60 inches wide. Apertures may be formed by the wire mesh construction shown in FIG. 3B or may be narrow slits as in expanded pressed steel . In either case the apertures need to be small enough in at least one dimension to prevent pieces of wood having small cross section from falling out of the basket through the apertures .
  • the wood to be processed has a maximum cross section to ensure that all of the wood is fully cooked in the fixed immersion time that the apparatus is designed to provide.
  • FIG. 3D shows the basket carrier of the embodiment of FIG. 1, and pivot bar 32 and pivot plate 37 which together define a pivot axis within reactor bath 19.
  • pivot bar end 33 extends though side wall 28 and pivot plate 37, and is attached to the lower end of basket carrier lever 36.
  • Pivot plate 37 provides a pressure seal bearing to maintain the integrity of reactor vessel 20.
  • basket carrier actuator cylinder 34 pulls basket carrier drive rod 35 down so as to rotate basket carrier lever 36 and basket 30 about the pivot axis.
  • FIG. 3D also shows the basket having apertures 38.
  • pivot bar 32 may be supported by a pivot plate wholly within the reactor bath and a rotational drive may be detachably coupled to pivot bar 32 only while the lid is retracted.
  • reactor 20 has a double wall
  • the double wall substantially surrounds the reactor. Gas given off in the reactor during the reaction phase flows through wall conduit 23, thereby providing thermal insulation for the molten tin in the reactor.
  • reservoir 50 which stores molten tin for use in the reactor.
  • Reservoir 50 has a supply conduit 51 coupled to supply molten tin to the reactor via inlet conduit 26.
  • Reservoir 50 also has a return conduit 52 coupled to accept molten tin from outlet conduit 27 of the reactor.
  • reservoir 50 has a first compartment 56 coupled by check valve 107 to a second compartment 57, a pressurized air inlet 54, and a controllable vent 55.
  • the top of reservoir 50 is approximately three feet below the base of reactor 20.
  • Reservoir 50 also has a corrugated bottom heat exchanger 53, and an excess air heater 60 for heating the molten tin in the reservoir.
  • Heater 60 has a fuel supply line 61, and an air blower 62 set for a 10:1 ratio, air to gas, at the burner.
  • Hot gas enters heat exchanger 53 at a temperature above 480°C, and leaves at a temperature in the range 310-320°C via excess-air heater flu 63.
  • a first portion of the gas from flu 63 supplies heat to steam generator 70.
  • Steam generator 70 supplies quenching steam to the reactor during the quenching phase via steam conduit 71.
  • the steam generator receives water from water supply 72, and heat from a first portion of hot gas from flu 63.
  • Exhaust from the steam generator at a temperature of approximately 260°C is vented via flu pipe 73.
  • a second portion of hot exhaust gases passing through flu 63 is vented via bypass flu pipe 74 and flu pipe 73, under control of flu pipe control valve 75.
  • Valve 75 is used to stabilize the temperature of hot gas entering the steam generator.
  • Condenser 80 condenses reactor gas given off in the reactor during the reaction phase.
  • the condenser accepts gas from reactor gas outlet 25 via gas inlet 81, and delivers hydrocarbon condensate to collection tank 90.
  • Collection tank 90 is coupled to supply fuel to excess air heater 60 via combustible gas outlet 91 and fuel supply line 61.
  • the condenser includes a particulates trap (not shown) and a pressure region of about 1" water below atmospheric pressure. Liquids leave the condenser via liquids drain 92.
  • FIG. 1 shows the distillation unit in the reaction phase of a batch thermolytic distillation cycle.
  • the previous batch cycle ends with the lid retracted, as illustrated in FIG. 3A, the char from the previous cycle having been discharged onto the conveyor system, as illustrated in FIG. 5.
  • a preferred process for batch thermolytic distillation of carbonaceous material proceeds as follows.
  • basket carrier 31 moves porous basket 30 from its tipped position (the upper position shown in FIG 5) to its operational position inside reactor 20. To do this, basket carrier 31 rotates the basket about a pivot axis defined by pivot bar 32 so the basket moves along arc B-B of FIG. 5. Then, as shown in FIG. 4, a charge of wood 100 is pushed by bulldozer or other means into basket 30. With the charge of wood in the basket, lid carrier 41, shown in FIG. 3B, moves lid
  • Tin Flow Filling, Maintaining and Emptying the Reactor Reactor 20 is filled with molten tin from reservoir compartment 56 by application of air pressure to the surface of the tin within reservoir compartment 57.
  • Molten tin returns from the reactor to the reservoir either by gravity or by application of steam pressure to the surface of the tin within the reactor.
  • the reactor fills in approximately 60 seconds.
  • the process of filling, maintaining and draining the reactor is illustrated in FIGS. 1 and 6. Referring to FIG. 6, the initial settings and sequencing of the tin flow valves is as listed in Table 1 below.
  • liquid tin is pressurized from air injected into first compartment 56, through valve 102. Liquid tin flows past check valve 106 and into the reactor. Tin fills up the reactor and overflows through pipes into second compartment 57, past check valve 108. Compartment 57 is vented through valve 104.
  • Check valve 107 stops tin flow into compartment 57 while under pressure.
  • valves 101-105 are set as above and liquid tin is pressurized in compartment 57.
  • Check valve 108 holds.
  • Check valve 106 holds.
  • Check valve 107 allows flow from compartment 57 to compartment 56.
  • valves change and flows are as described in A.
  • a & B repeat until charge in reactor has been immersed in high temperature for 15 minutes.
  • valves 101-105 are set as above and tin flows from the full reactor back through fill pipe by gravity, through valve 105, through check valve 108, into compartment 57, and through check valve 107 into compartment 56.
  • actuators 48 push the lid up, and motor 45 translates the lid horizontally
  • the char in the basket is now cool enough to be tipped onto the belt conveyor system (FIG. 5) .
  • the fluids are further separated into water, combustible gases, combustible liquids and tars.
  • gas leaving reactor 20 exits downward via gas outlet slots 24, and wall conduits 23 between the double walls of the reactor.
  • the gas then passes through rector gas outlet 25 and is received by condenser 80 at reactor gas inlet 81.
  • the gas is condensed in condenser 80 as distillate (wood-petrol) and other condensable products.
  • wood-petrol collects in tank 90.
  • Wood petrol from tank 90 is separated into a light fraction, a heavy fraction, and non-condensed combustible gas in a distillation column (not shown) within the condenser. Some or all of the combustible gas is burned in excess air heater 60 to maintain the proper temperature of molten tin in reservoir 50.
  • Wall conduits 23 in the end walls of reactor 20 are shown in FIG. 1.
  • Wall conduits 23 in side walls 28 of reactor 20 are shown in FIG. 3D. These conduits provide a passage for vapor produced by thermolysis.
  • the double- wall structure of the reactor bath significantly reduces heat loss from the molten tin.
  • Heating the Reservoir Reservoir 50 includes corrugated bottom 59, shown in FIG. 7B, which serves as part of heat exchanger 53, shown in FIG. 1.
  • the corrugated bottom significantly increases heat exchange surface area and facilitates heat transfer between the hot gases from excess air heater 60, shown in
  • FIG. 7A and the molten tin in the reservoir.
  • the corrugated bottom also provides the strength needed to support the enormous weight of a bath of molten tin.
  • excess air heater 60 includes air blower 62, duct 67, fuel supply line 61, and perforated pipe 65, the perforated pipe having a plurality of nozzles 66. Arrows in FIGS. 7A and 7B show
  • excess air heater 60 may be fueled by auxiliary fuel via auxiliary fuel supply line 64 shown in FIG. 1.
  • Molten tin is used at a temperature of approximately 851°F (455°C) .
  • the depth of the tin in the reactor is 30 inches.
  • the basket is 60 inches long, 36 inches deep and 60 inches wide, i.e. 62.5 cubic feet per basket. Wood having a maximum cross section of one inch is loaded into the basket . Wood is immersed for a predetermined immersion time of 10 minutes. This is sufficient to fully cook wood having a smallest cross section no greater than one inch.
  • Tar for analysis was collected from a vapor exit pipe above the baskets.
  • the material is a bituminous oil consisting of a mixture of heavy hydrocarbons

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Coke Industry (AREA)

Abstract

L'invention concerne une unité de distillation pour la distillation thermolytique discontinue de matière carbonée en blocs se prêtant à un montage côte à côte d'unités multiples. L'unité est dotée d'un bain réacteur contenant de l'étain fondu à une température d'environ 455 °C, d'un couvercle rétractable présentant un collier de fixation hydraulique, d'un réservoir de stockage de l'étain fondu et d'un panier monté rotatif dans le bain réacteur. Le couvercle comprend une paroi périphérique et un écran perforé. Un procédé de distillation discontinue thermolytique de matière carboné en blocsen blocs consiste à faire tourner autour d'un axe traversant le bain réacteur un panier; à mettre une charge de bois dans le panier ; à fermer le couvercle rétractable sur le bain réacteur ; à remplir ledit bain d'une matière fondue pour obtenir du gaz et du charbon par conversion thermolytique de la charge, en purgeant le bain de matière fondue alors que le couvercle est fermé ; à tremper le charbon dans le bain réacteur avec le courant ; à ouvrir le couvercle et finalement à retirer le charbon du panier.
PCT/US1999/030002 1999-01-27 1999-12-22 Distillation discontinue thermolytique de matiere carbonee Ceased WO2000044854A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US11738099P 1999-01-27 1999-01-27
US60/117,380 1999-01-27

Publications (1)

Publication Number Publication Date
WO2000044854A1 true WO2000044854A1 (fr) 2000-08-03

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015171865A1 (fr) 2014-05-09 2015-11-12 Academia Sinica Système et procédé de supertorréfaction en discontinu
CN109575969A (zh) * 2018-12-27 2019-04-05 上海大学 一种简单无氧热解制备生物炭的方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4925532A (en) * 1989-04-24 1990-05-15 Pto, Inc. Apparatus for thermal conversion of organic matter
EP0592057A1 (fr) * 1992-10-06 1994-04-13 FORMEX TRADING GmbH Procédé de pyrolyse de déchets organiques
US5704557A (en) * 1995-03-06 1998-01-06 Eli Eco Logic Inc. Method and apparatus for treatment of organic waste material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4925532A (en) * 1989-04-24 1990-05-15 Pto, Inc. Apparatus for thermal conversion of organic matter
EP0592057A1 (fr) * 1992-10-06 1994-04-13 FORMEX TRADING GmbH Procédé de pyrolyse de déchets organiques
US5704557A (en) * 1995-03-06 1998-01-06 Eli Eco Logic Inc. Method and apparatus for treatment of organic waste material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015171865A1 (fr) 2014-05-09 2015-11-12 Academia Sinica Système et procédé de supertorréfaction en discontinu
EP3140370A4 (fr) * 2014-05-09 2017-12-27 Academia Sinica Système et procédé de supertorréfaction en discontinu
CN109575969A (zh) * 2018-12-27 2019-04-05 上海大学 一种简单无氧热解制备生物炭的方法

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