CN1507528A - In-situ combustion for oil recovery - Google Patents
In-situ combustion for oil recovery Download PDFInfo
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- CN1507528A CN1507528A CNA018232906A CN01823290A CN1507528A CN 1507528 A CN1507528 A CN 1507528A CN A018232906 A CNA018232906 A CN A018232906A CN 01823290 A CN01823290 A CN 01823290A CN 1507528 A CN1507528 A CN 1507528A
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- reaction zone
- heat
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- stratum
- oxidant
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- 238000002485 combustion reaction Methods 0.000 title description 16
- 238000011084 recovery Methods 0.000 title description 5
- 238000011065 in-situ storage Methods 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 86
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 65
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 61
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 60
- 230000001590 oxidative effect Effects 0.000 claims abstract description 42
- 239000007800 oxidant agent Substances 0.000 claims abstract description 36
- 238000002347 injection Methods 0.000 claims abstract description 34
- 239000007924 injection Substances 0.000 claims abstract description 34
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000567 combustion gas Substances 0.000 claims abstract 15
- 239000012530 fluid Substances 0.000 claims description 110
- 239000000446 fuel Substances 0.000 claims description 43
- 238000000197 pyrolysis Methods 0.000 claims description 13
- 239000004058 oil shale Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000003245 coal Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 4
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- 238000013508 migration Methods 0.000 abstract 1
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- 230000003647 oxidation Effects 0.000 description 143
- 238000010438 heat treatment Methods 0.000 description 42
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 239000000571 coke Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
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- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
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- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 2
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- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- BGOFCVIGEYGEOF-UJPOAAIJSA-N helicin Chemical group O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=CC=C1C=O BGOFCVIGEYGEOF-UJPOAAIJSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
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- 239000004576 sand Substances 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
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- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000013529 heat transfer fluid Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
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- 239000011707 mineral Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B36/00—Heating, cooling or insulating arrangements for boreholes or wells, e.g. for use in permafrost zones
- E21B36/02—Heating, cooling or insulating arrangements for boreholes or wells, e.g. for use in permafrost zones using burners
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B36/00—Heating, cooling or insulating arrangements for boreholes or wells, e.g. for use in permafrost zones
- E21B36/04—Heating, cooling or insulating arrangements for boreholes or wells, e.g. for use in permafrost zones using electrical heaters
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
- E21B43/24—Enhanced recovery methods for obtaining hydrocarbons using heat, e.g. steam injection
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
- E21B43/24—Enhanced recovery methods for obtaining hydrocarbons using heat, e.g. steam injection
- E21B43/2401—Enhanced recovery methods for obtaining hydrocarbons using heat, e.g. steam injection by means of electricity
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
- E21B43/24—Enhanced recovery methods for obtaining hydrocarbons using heat, e.g. steam injection
- E21B43/243—Combustion in situ
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Mining & Mineral Resources (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Resistance Heating (AREA)
- Pipe Accessories (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
- General Induction Heating (AREA)
- Lubricants (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Incineration Of Waste (AREA)
- Mounting, Exchange, And Manufacturing Of Dies (AREA)
- Bridges Or Land Bridges (AREA)
- Exhaust Gas After Treatment (AREA)
- Perforating, Stamping-Out Or Severing By Means Other Than Cutting (AREA)
- Earth Drilling (AREA)
- Feeding And Controlling Fuel (AREA)
- Control Of Electric Motors In General (AREA)
- Fats And Perfumes (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
- Liquid Developers In Electrophotography (AREA)
Abstract
A method and system for transmitting heat substantially by conduction into a hydrocarbon containing formation surrounding a heat injection well utilise oxidant supply and combustion gases exhaust conduits disposed in the wellbore of the heat injection well, wherein an oxidant, such as air, in injected through the oxidant supply conduit to a reaction zone in the formation in the vicinity of the heat injection well where at least a portion of the hydrocarbons in the formation are oxidized such that heat and combustion gases are generated, and at least a portion of the combustion gases are transmitted through the combustion gases exhaust conduit away from the reaction zone such that migration of combustion gases from the reaction zone into the hydrocarbon containing formation is inhibited.
Description
[background of invention]
The present invention relates to a kind of heating ring that is used for around for example coal seam of heat injection well or the method and apparatus on the stratum of containing hydrocarbon of oil shale deposit thing.
Application to the oil shale formation heating has been described in the United States Patent (USP) 4886118 of the United States Patent (USP) 2923535 of Ljungstrom and Van Meurs etc.These prior art lists of references disclose electric heater with the heat transferred oil shale formation, thereby make the oil bearing rock pyrolysis in the oil shale formation.This heat also can make this stratum breaking, to increase the permeability on this stratum.The permeability that increases allows formation fluid to advance in the recovery well, takes this fluid here from this oil shale formation away.For example, in the disclosed certain methods of Ljungstrom, from a preheating step, the gas medium that contains oxygen is preferably in and is introduced into permeable stratum when still awfully hot, to take fire.
United States Patent (USP) 2548360 has been described the electrical heating elements in a kind of viscous oil that is placed in the pit shaft.This heating element is with the oil heating and make it thinning, thereby allows pump oil from pit shaft.United States Patent (USP) 4716960 has been described a kind of pipe-line system that flows through oil well by the electric current that makes relatively low pressure and has been come it is carried out electrical heating to prevent the formation of solid.The United States Patent (USP) 5065818 of Van Egmond has been described and a kind of it has been bonded in electrical heating elements in the pit shaft with cement, and need not be around the sleeve pipe of this heating element.
The United States Patent (USP) 6023554 of Vinegar etc. has been described a kind of electrical heating elements that is positioned at sleeve pipe.This electrical heating elements produces the emittance of heating muff.Granular solid filler matter can be arranged between sleeve pipe and this stratum.Sleeve pipe can heat filler with conducting, then this stratum of conduction ground heating.
United States Patent (USP) 4570715 as Van Meurs of all openly being combined in this with reference to it etc. has been described a kind of electrical heating elements.This heating element has conductive core, the embracing layer of being made by insulation materials and the protective metal shell that centers on.This conductive core can have at high temperature relatively low resistance.This insulation materials can have at high temperature higher relatively resistance, compressive strength and heat conductivility.This insulating layer can prevent to form arcing from the fuse to the protective metal shell.This protective metal shell can have at high temperature higher draw tensile strength and creep resistance relatively.
As having described a kind of electrical heating elements with corronil fuse with reference to its United States Patent (USP) 5060287 that all openly is combined in this Van Egmond.
Also can use the burning of fuel to heat the stratum.Combustion fuel heats the stratum than using electric energy heating stratum more economically.Several multi-form heaters can use the thermal source of fuel combustion as the heating stratum.Can be in the stratum, burn in the well and/or near the place on surface.
United States Patent (USP) 4662443,4662439 and 4648450 discloses the fire flooding of the hydrocarbon of burning in subsurface formations, and wherein for example the oxidant of air pumps in this stratum.Oxidant can be lighted so that advanced towards recovery well in the flare front portion.The oxidant that pumps in this stratum can flow through this stratum along the geosutures in this stratum.Lighting of oxidant can not make the flare front portion pass through the stratum equably.
Also know, can use aphlogistic burner to burn and inject the fuel of heated well.Seem with reference to they whole openly be combined in this Mikus United States Patent (USP) 5255742, Vinegar etc. 5404952,5862858 and the Wellington etc. of Wellington etc. 5899269 the non-flaming combustion device has been described.Arrive the temperature that is higher than the automatic ignition temperature of this mixture by heating fuel and combustion air in advance, can finish non-flaming combustion.Fuel and combustion air are mixed so that burning.In the thermal treatment zone of non-flaming combustion device, catalytic surface can be set to reduce the automatic ignition temperature of fuel and air mixture.In these known non-flaming combustion devices, by the supply line that separates fuel and oxidant are injected in the heated well, perhaps by unique supply line supplying mixed compound, waste gas then is discharged into ground by discharge tube, and this discharge tube can surround fuel and/or oxidant supply line coaxially.
Also known and supplied heat to the stratum from the ground heater.This ground heater can produce burning gases, makes burning gases flow through pit shaft so that the heating stratum.Form of implementation can use the ground stove to heat heat transfer fluid as an alternative, and it heats the stratum through pit shaft.The United States Patent (USP) 6056057 of Vinegar etc. and Mikus etc. 6079499 in illustration can be used for the ignition heater or the ground stove of sub-surface heatedly, seem openly to be combined in this with reference to the whole of them.
The shortcoming that fuel, oxidant and/or waste gas flow through the heater of the known ground of heated well and down-hole is: the housing in the heated well and other pipelines need be made by resistant to elevated temperatures steel grade, and especially housing bears the high extruding force that is caused by the thermal expansion around the stratum.Therefore, the sleeve pipe in heated well must be by the high temperature resistant and corrosion resistant stainless steel manufacturing of costliness.If it is installation electric heater, the supply of fuel and the supply of electric energy also need complicated substructure usually, therefore relatively more expensive.
The shortcoming of known fire flooding is: produce the crack in irregular mode in containing the stratum of hydrocarbon, and have only near the hydrocarbon the crack oxidized, so can only heat these stratum in quite irregular and out of contior mode.
The objective of the invention is to subdue known fire flooding, inject the shortcoming of fuel combustion and electrical heating method, and a kind of heating means and device of down-hole of cheapness are provided, its in uniform mode with in check heat transferred stratum.
[summary of the invention]
According to the present invention, be used for the device of heat transferred around the stratum of containing hydrocarbon of heat injection well comprised:
The oxidation fluid source;
Be arranged in the oxidant supply line in the heat injection well shaft, wherein this pipe configuration is for during use can be from this oxidation fluid source being fed to oxidation fluid the reaction zone the stratum, and this oxidation fluid is selected to can be during use with at least a portion hydrocarbon oxidation near stratum shaft area, thereby produces heat at this reaction zone;
Be arranged in the burning gases discharge tube in the heat injection well shaft, the pit shaft that is used for by this heat injection well is sent to place away from reaction zone with burning gases.
Preferably make this device construction become to allow during use heat to be sent to the selected district on stratum basically from reaction zone by conduction.
Preferably this oxidant supply line and burning gases discharge tube are provided with regulator, this regulator is controlled at the pressure in the reaction zone, thereby can will be discharged into ground at sizable at least a part of burning gases that reaction zone produces by the burning gases discharge tube.
In some cases, this pressure-generating device can be used for allowing a part of burning gases to be discharged into ground, and allows a part to penetrate this treatment region.Can make the interior pressure ratio of pit shaft away from the pressure height in the shaft area like this.This pressure reduction can make oxidation fluid arrive reaction zone quickly and/or with more amount ground, thereby allows to produce the heat that increases by this reaction zone.
Comparatively suitable is, oxidant flow in pipes and burning gases discharge tube extend into the stratum of containing hydrocarbon from the well head of heated well coaxially to each other, and this oxidant flow in pipes stretches out from the lower end of oxidant flow in pipes and penetrates into less the stratum that a sizable part contains hydrocarbon, and the bottom of the oxidant flow in pipes that stretches out is provided with a row oxidant inlet, is injected in the annular space between oxidant flow in pipes and reaction zone with subsonic speed or ultrasonic speed by these inlets oxidant wherein.
This oxidant flow in pipes can be the air injection tube road and be provided with the air injection pump, each all can be provided with pressure-control valve air injection tube road and burning gases discharge tube, so that be controlled at the bottom and the interior pressure of the annular space between this reaction zone of the punching of this oxidant flow in pipes, thereby make described pressure be substantially equal to pore pressure in the stratum of containing hydrocarbon around at least a portion, and stop burning gases to be sent in the stratum.But in some cases, can allow burning gases partly to penetrate into the stratum, so that the accelerating oxidation fluid is sent to reaction zone and is increased in the heat that the there produces.
The fuel flow in pipes perhaps is equipped with in order to start or to support combustion (of oil) insitu process, this heated well electric heater can be equipped with, so that other fuel is injected into reaction zone so that with the heat transferred reaction zone.
[description of drawings]
By example the present invention is described in further detail below with reference to accompanying drawing, wherein:
Fig. 1's embodiment of combustor heat source of NATURAL DISTRIBUTION has drawn;
The drawn tectal part on stratum of Fig. 2 with thermal source;
Fig. 3's embodiment of combustor heat source of NATURAL DISTRIBUTION and 4 has drawn;
Fig. 5's embodiment of the device that is used for heating the stratum and 6 has drawn.
[detailed description of invention]
According to the present invention, in the stratum of heat injection well, heat the stratum of containing hydrocarbon by the oxidation on the spot of hydrocarbon, this device is also referred to as burner (NDC) heater of NATURAL DISTRIBUTION.The heat that can allow to produce passes to around the part on the stratum of heated well by convection current, thereby is heated, but stops or partly stop burning gases to be sent to the stratum from reaction zone.
Be enough to support that the temperature of oxidation can be for example about at least 200 ℃ or 250 ℃.Yet, be enough to support that the temperature of oxidation trends towards changing according to the composition of the hydrocarbon in the stratum of for example containing hydrocarbon.Before heating, can from the stratum, remove moisture.For example, can use dewatering well from the stratum, to aspirate moisture.The part that is heated on this stratum can the approaching or contiguous basically opening in containing the stratum of hydrocarbon.This opening in the stratum can be formed in the heated well in the stratum.Can form heated well according to arbitrary form of implementation described here.Contain hydrocarbon the stratum be heated part diametrically can from opening extend to about 0.3 meter to about 1.2 meters width.Yet this width also can be less than about 0.9 meter.The width that is heated part can change.For example in certain embodiments, this change depends on that producing enough heats between carbon period need not provided heat needed width to keep oxidation reaction by other thermal source.
This part on stratum reach be enough to support the temperature of oxidation after, can infeed this opening to oxidation fluid, so that the reaction zone of oxidation in the stratum or at least a portion hydrocarbon in thermal source district.The oxidation of this hydrocarbon will produce heat at reaction zone.In most embodiment, the heat of generation will pass to pyrolysis zone the stratum from reaction zone.In certain embodiments, the heat of generation transmits with the ratio of measuring along the degree of depth of this reaction zone between every meter about 650 watts to 1650 watts.Because the oxidation of at least some hydrocarbon in the stratum, so can reduce or can close to be used for initial heating and the energy of supply heater.Like this, can significantly reduce energy input expense, more effectively be used for heating significantly the device on stratum thereby provide.
In one embodiment, can be pipe arrangement in this opening, so that oxidation fluid is supplied with this opening.This pipeline can have metering orifice or other flow control device (being otch, venturi meter, valve etc.), enters this opening to allow oxidation fluid.Term " hole " comprises the opening with shape of cross section variation widely, and these shapes include but not limited to shape circle, ellipse, square, rectangle, triangle, slit or other rules or irregular.These metering orifices can be critical flow orifice, fluid with at a high speed for example ultrasonic velocity flow through this hole so that the oxidation fluid of the basically identical flow being provided for this opening, and no matter the pressure size in this opening.
In certain embodiments, be formed in the pipeline or be connected to the metering orifice on the pipeline quantity can by the diameter in these holes and for the length of pipeline the needs between these holes limit at interval.For example, along with the diameter in these holes reduces, the quantity of metering orifice can increase, and vice versa.In addition, along with needs increasing at interval, the quantity of metering orifice can increase, and vice versa.For example can determine the diameter in these holes by the pressure in the pipeline and/or by the flow velocity that needs in these holes.For example, for the flow of about 1.7 standard cubic meters of per minute and about 7 crust absolute pressures, the diameter in hole can be about 1.3mm, is spaced apart about 2m between these holes.
For example because fluid dirt in opening or in these holes or from the influence of the near solid deposits of these Kongzuis, so stop up than the larger-diameter Kong Gengyi of the boring ratio of minor diameter.In certain embodiments, can select the quantity and the diameter in these holes, so that the depth of stratum in this opening obtains more evenly or approaching consistent heating profile.For example, being intended that the degree of depth that is heated the stratum that has near consistent heating profile can be greater than about 300m, even greater than about 600m.Yet such degree of depth can change, and it for example depends on the kind on stratum to be heated and/or the productivity ratio of needs.
In certain embodiments, metering orifice can be with spiral helicine form around the pipeline setting in this opening.These metering orifices can arrive about 3m with spiral helicine form at interval about 0.3m between the hole.In certain embodiments, this can for example be about 1.5m for about 1m arrives about 2m at interval.
Can control the flow velocity that flows into the oxidation fluid in this opening, thereby make in the oxidation rate of reaction zone controlled.Oxidation fluid also can cooling pipe, thereby makes that this pipeline basically can be not oxidized and heat.
Fig. 1 shows the embodiment of the burner of the NATURAL DISTRIBUTION that is configured to be used for heating the stratum of containing hydrocarbon.Pipeline 512 can be arranged in the opening 514 on stratum 516.Pipeline 512 can have interior conduit 513.Oxidation fluid source 508 can be supplied with interior conduit 513 to oxidation fluid 517.Interior conduit 513 can have critical flow orifice 515 along its length.Critical flow orifice 515 can be arranged with spiral form (perhaps any other forms) along the length of the interior conduit 513 in the opening 514.For example, can between adjacent holes, arrange critical flow orifice 515 to the distance of about 2.5m with the form of spiral at a distance of about 1m.Can further form critical flow orifice 515 according to form described here.Interior conduit 513 is sealed in the bottom.The critical flow orifice 515 of passing interior conduit 513 can be fed to oxidation fluid 517 in the opening 514.
Encapsulant 542 can fence up the pipeline 512 in the covering layer 540 on stratum.Encapsulant 542 can stop basically fluid from opening 514 to ground 550 flow.Encapsulant 542 can comprise can be configured to stop fluid 550 material that flows, for example cement, sand and/or blindings earthward arbitrarily.
Oxidation product 519 enters pipeline 512 from opening 514 usually.Oxidation product 5 19 can comprise carbon dioxide, nitrogen oxide, sulfur oxide, carbon monoxide and/or be reacted and other products of producing by oxygen and hydrocarbon and/or carbon.Can oxidation product 519 be discharged into ground 550 by pipeline 512.Oxidation product 519 can be moving along the surface current of the reaction zone in opening 514 524, near arriving opening 514 tops of oxidation product 519 in can flow ipe 512.Also can discharge oxidation product 519 by the pipeline and/or a plurality of pipeline that are arranged in opening 514 and/or the stratum 516.For example, can discharge oxidation product 519 by second pipeline that is arranged in the opening 514.Discharge oxidation product 519 by pipeline and can prevent basically that oxidation product 519 from flowing in the recovery well that is arranged in the stratum 516.Critical flow orifice 515 also can be constructed to be permeable to stop oxidation product 519 to enter interior conduit 513 basically.
The flow velocity of oxidation product 519 can balance each other with the flow velocity of oxidation fluid 517, thereby keeps the pressure of substantial constant in opening 514.The part that is heated for 100m length, the flow velocity of oxidation fluid can be at about 0.5 standard cubic meter per minute between about 5 standard cubic meter per minutes, perhaps arriving between about 4 standard cubic meter per minutes at about 1.0 standard cubic meter per minutes, perhaps for example is 1.7 standard cubic meter per minutes.For example, the pressure in opening can be about 8 crust absolute pressures.Oxidation fluid 517 can reaction zone 524 oxidations contain hydrocarbon stratum 516 be heated at least a portion hydrocarbon in the part 518.Use as shown in Figure 5 electric heater or other suitable device or methods arbitrarily described here, beginning is heated the temperature that part 518 is heated to is enough to support oxidation to this.In certain embodiments, electric heater can be arranged in the inside of pipeline 513 or be bundled into the outside of pipeline 513 with belt.
In certain embodiments, the pressure in the control opening 514 is useful, thereby can stop oxidation product and/or oxidation fluid to flow into the pyrolysis zone on stratum.In some cases, pressure in opening 514 and the pressure in the stratum balance each other, so that reach such effect.In other embodiment, can allow some combustion products to flow in the stratum, so that the pressure reduction that produces makes oxidation fluid add the flow speed and direction reaction zone like this, improve hot generation rate thus.
Though, can stop basically that oxidation product 519 (and excessive oxidation fluid, for example air) is mobile to be passed this stratum and/or flow to recovery well in stratum 516 the heat transferred stratum that oxide produces.But as described herein such, oxidation product 519 (and excessive oxidation fluid) is removed (for example by pipeline, such as pipeline 512).In this manner, oxidation and with the heat transferred stratum can stop basically and/or partly or completely prevent that pyrolysis zone is exposed to oxidation product 519 and/or oxidation fluid simultaneously.
In certain embodiments, also can be near reaction zone 524 oxidations some thermal decomposition products except carbon reaction zone 524.The oxidation of thermal decomposition product can provide other heating to stratum 516 in reaction zone 524.When this oxidation of thermal decomposition product takes place, need be according to described here such, near reaction zone, remove the oxidation product that (for example by pipeline, such as pipeline 512) produces owing to this oxidation, thereby stop this oxidation product pollution other thermal decomposition products in this stratum.
The openings 514 that pipeline 512 can be constructed to be permeable to from the stratum in 516 are removed oxidation products 519.Like this, from the oxidation product 519 in the pipeline 512, can heat oxidation fluid 517 in interior conduit 513 by the interchange of heat in covering layer part 540.By with heat transferred oxidation fluid 517, can cool off oxidation product 519.In this manner, the oxidation of the hydrocarbon in stratum 516 can have the thermal efficiency more.
Oxidation fluid 517 can pass reaction zone 524 or the thermal source district transmits by gas phase diffusion and/or convection current.Under the relatively-high temperature of oxidation, oxidation fluid 517 passes the diffusion of reaction zone 524 can be more effective.The diffusion of oxidation fluid 517 can be suppressed at the hot-spot in this stratum and the development of finger-like phenomenon.Pass normally a kind of mass transfer process of diffusion of the oxidation fluid 517 on stratum 516.Do not having under the situation of external force, the diffusion velocity of oxidation fluid 517 depends on concentration, pressure and/or the temperature of the oxidation fluid 517 in stratum 516.This diffusion velocity depends on that also oxidation fluid 517 passes the diffusion coefficient on stratum 516.This diffusion coefficient can be definite by measuring, and perhaps calculates based on the theory of molecular motion of gas.Usually, the random motion of oxidation fluid 517 can be sent to low concentration region to oxidation fluid 517 from area with high mercury through stratum 516.Flow through the principle of porous media according to fluid, control the convection current of oxidation fluid from the injection hole to the reaction zone by the pressure reduction between pit shaft and reaction zone.
As time goes by, because hydrocarbon is oxidized, reaction zone 524 can be from opening 514 slow leading threads to expanding to bigger diameter.In many examples, reaction zone 524 can keep constant relatively width.For example, for the stratum of containing hydrocarbon, reaction zone 524 can be with the velocity radial ground expansion less than about 0.91 meter every year.For example, for the stratum that comprises the coal seam, reaction zone 524 can be expanded to the velocity radial ground between about 1 meter every year with about 0.5 meter every year.For the stratum of containing oil shale, reaction zone 524 can with 1 year about 2m and time afterwards according to lower velocity radial ground expansion, this is because along with the reason of the increase of the volume of the radial expansion reaction zone 524 of reaction zone 524.This lower speed can be about 1 meter every year to about 1.5 meters every year.For the abundant stratum (for example coal) of hydrocarbon, reaction zone 524 can be with lower speed expanded, and the stratum that has more inorganic material for wherein (for example oil shale), can expand with fast speeds, because in the stratum that hydrocarbon enriches, per unit volume can obtain more hydrocarbon and be used for burning.
Along with the diameter of reaction zone 524 increases, can improve oxidation fluid 517 and enter flow velocity in the opening 514, thereby the oxidation rate of per unit volume is remained on basicly stable state.Therefore in certain embodiments, the temperature in reaction zone 524 can remain substantially constant.Temperature in reaction zone 524 can for example be about 760 ℃ between about 650 ℃ to about 900 ℃.
Temperature in reaction zone 524 can change, and for example it depends on the firing rate of selected part 526 needs.Enter flow velocity in the opening 514 by improving or reduce oxidation fluid 517 respectively, can raise or be reduced in the temperature in the reaction zone 524.Yet the temperature of pipeline 512, interior conduit 513 and/or any metallurgical material in opening 514 can not surpass the temperature that begins to make quick distortion of this metallurgical material or corrosion usually.
The diameter increase of reaction zone 524 can be heated the stratum 516 of containing hydrocarbon relatively quickly.Along with the increase of the diameter of reaction zone 524, the heat that time per unit produces in reaction zone 524 also can increase.In many cases, the heat increase that time per unit produces in reaction zone 524 will can be provided in the firing rate that improve on stratum 516 in a period of time, though can not improve in reaction zone temperature or in the temperature at pipeline 513 places.Can obtain the heat of increase along with the past of time like this, and other thermal source need not be installed, and can not improve temperature.In certain embodiments, firing rate can improve, and allowable temperature descends (life-span that allowable temperature decline often can prolong use equipment) simultaneously.
By the carbon in the stratum is used as fuel, the burner of this NATURAL DISTRIBUTION is the energy conservation expense significantly.Therefore can provide a kind of method of economy for layer heatedly, otherwise, heat improper economically with additive method.Also have, seldom having heaters can be placed on the area of expansion on stratum 516.This also provides the equipment cost of the reduction relevant with heating stratum 516.
Can pass to the selected part 526 on stratum 516 by conduction of heat at the heat of reaction zone 524 generations.In addition, the heat of generation can be delivered to selected part by convection current from reaction zone in less degree ground.Sometimes be also referred to as " pyrolysis zone " in this selected part 526, its contiguous basically reaction zone 524.Because remove oxidation product (and excessive oxidation fluid, for example air) from this reaction zone usually,, and can not be subjected to the oxidation product in reaction zone or the influence of oxidant so pyrolysis zone can receive heat from reaction zone.If oxidation product and/or oxidation fluid are present in the pyrolysis zone, they can cause forming unwanted stratum product so.For example, need under reducing environment, carry out pyrolysis in certain embodiments.Therefore, allow heat to be delivered to pyrolysis zone and to stop or prevent that oxidation product and/or oxidation fluid from arriving pyrolysis zone often is useful from reaction zone.
The process of the pyrolysis or the control of other heats of hydrocarbon can take place in heated selection area 526.Selection area 526 can be in the temperature between about 270 ℃ to about 400 ℃, so that pyrolytic.Can the raise temperature of selection area 526 of the heat transmission in origin autoreaction district 524.As arbitrary embodiment described here is described, the speed that can select temperature to raise.Can be controlled in the stratum 516, select the temperature in part 526 and/or the reaction zone 524, thereby can stop the generation of nitrogen oxide basically.Usually produce nitrogen oxide being higher than under about 1200 ℃ temperature.
Can monitor temperature in opening 514 with being placed on thermocouples in the opening 514.Can monitor the temperature in opening 514, thereby temperature is remained in the selected scope.Should selected scope can change, for example depend on the firing rate of stratum 516 needs.Temperature can be remained in the selected scope by the flow velocity that improves or reduce oxidation fluid 517.For example,, can improve the flow velocity of oxidation fluid 517 so, so that increase burning and so the temperature of raising in opening 514 if the temperature in opening 514 drops under the selected temperature scope.Form of implementation as an alternative, thermocouple can be arranged on the pipeline 512 and/or be placed on the face of reaction zone 524, thereby can monitoring temperature.
In certain embodiments, can arrange one or more natural distributed combustor along the direction of strata and/or horizontal direction.Do the pressure reduction that will certainly reduce like this, thereby help lend some impetus to the control of uniform heating and improvement more along the heated length of this well.
In certain embodiments, can monitor the existence of air in oxidation product 519 or molecular oxygen, oxygen.Form of implementation can be monitored nitrogen, carbon monoxide, carbon dioxide, nitrogen oxide, sulfur oxide equal size in oxidation product 519 as an alternative.The composition and/or the amount of monitoring oxidation product 519 all are useful for heat balance, process diagnosis, process control etc.
Fig. 2 shows the tectal embodiment of a part that has the natural distributed combustor described in Fig. 1.Covering layer sleeve pipe 541 can be arranged in the covering layer 540 on stratum 516.Can be with stoping material to covering layer 540 heating (for example thermal insulation material, such as cement) to surround covering layer sleeve pipe 541 haply basically.Covering layer sleeve pipe 541 can be by the metal material manufacturing, such as but not limited to carbon steel.
The covering layer sleeve pipe can be arranged in the strengthening material 544 in the covering layer 540.Strengthening material 544 for example can be cement, sand, concrete etc.Encapsulant 542 can be between covering layer sleeve pipe 541 and the opening in the stratum 514.Encapsulant 542 can be the material (for example cement, concrete, mortar etc.) of any atresia basically.Encapsulant 542 can stop fluid to flow to the outside of pipeline 512 and flow to opening 514 and ground 550 between.Interior conduit 513 can be delivered to fluid in the opening 514 in stratum 516.Pipeline 512 can be removed combustion product (perhaps excessive oxidation fluid) from the opening the stratum 516 514.The amount of the combustion product that produces according to the oxidation in this natural distributed combustor can be determined the diameter of pipeline 512.For example, the situation for produced relatively large exhaust combusted products by the NATURAL DISTRIBUTION burning heater just needs bigger diameter.
In an alternative embodiment, at least a portion stratum can be heated to such temperature, that is: at least a portion stratum of containing hydrocarbon can be changed coke or charcoal into.Coke and/or charcoal can be higher than the temperature about 400 ℃ and form down in higher firing rate (about for example greater than 10 ℃/day).Under the situation that oxidation fluid exists, coke or charcoal are with oxidized.As arbitrary embodiment described here, can produce heat by the oxidation of coke or charcoal.
Fig. 3 shows an embodiment of NATURAL DISTRIBUTION burning heater.Insulated electric conductor 562 can combine with pipeline 532 and be arranged in the opening 514 on stratum 516.Insulated electric conductor 562 can be arranged in the inside (thereby allow reclaim insulated electric conductor 562) of pipeline 532, and perhaps form of implementation as an alternative is combined in it on external surface of pipeline 532.Such insulated electric conductor for example can comprise mineral or pottery etc.In opening 514, pipeline 532 can have the critical flow orifice 515 of arranging along its length.Can such critical flow orifice 515 that forms as described herein.Electric current can be applied on the insulated electric conductor 562, so that in opening 514, produce radiant heat.Pipeline 532 can be constructed to the loop of electric current.Insulated electric conductor 562 can form and the part 518 of pressure reduction can be heated to the temperature that is enough to support the hydrocarbon oxidation.This part 518, reaction zone 524 and selected part 526 can have characteristic described herein.Such temperature can comprise temperature described herein.
Fig. 4 shows the embodiment of the NATURAL DISTRIBUTION burning heater of the fuel conductor that has increase.Fuel channel 536 can be arranged in the opening 514.In certain embodiments, it can be arranged in the place of adjacent conduit 533 in fact.In opening 514, fuel channel 536 can have critical flow orifice 535 along its length.In opening 514, pipeline 533 can have critical flow orifice 515 along its length.Can such critical flow orifice 515 that forms as described herein.Critical flow orifice 535 and critical flow orifice 515 can be arranged on fuel channel 535 and the pipeline 533, therefore fuel fluid of supplying with by fuel channel 536 and the oxidation fluid by pipeline 533 supplies basically can be owing to reaction heating fuel pipeline 536 and/or pipeline 533.For example, owing to contact with each other fuel fluid and oxidation fluid can react, thereby produce the heat that causes by reaction.The heat that causes owing to this reaction can be heated to such temperature with fuel channel 536 and/or pipeline 533, if that is: reaction occurs in from the nearest place of fuel channel 536 and/or pipeline 533, this temperature is enough to begin in fact to be melted in the metallurgical material in fuel channel 536 and/or the pipeline 533 so.Therefore, design arrangement is in critical flow orifice on the fuel channel 536 535 and the critical flow orifice on pipeline 533 515 like this, that is: from the nearest place of pipeline, this fuel fluid and oxidation fluid be Fails To Respond basically.For example, can pipeline 536 and 533 like this processing combine, that is: these holes are along opposite direction orientation, and these holes are towards the stratum 516.
The reaction of fuel fluid and oxidation fluid can produce heat.Can have some characteristics at this this fuel fluid and oxidation fluid.Fuel fluid for example can be natural gas, ethane, hydrogen or the forming gas that produces in the combustion (of oil) insitu process that the another part on stratum carries out.Can be set at the heat of this generation part 518 can be heated to the temperature that is enough to support the hydrocarbon oxidation.When part 518 being heated to when being enough to support the temperature of oxidation, can turning down or close the fuel stream that flows in the opening 514.Form of implementation can be supplied with fuel continuously in the heating process on whole stratum as an alternative, thereby utilizes the heat that stores in carbon that the temperature in the opening 514 is remained on the autoignition temperature of fuel.
Oxidation fluid can oxidation at least a portion hydrocarbon of reaction zone 524.The heat that produces is for example selected part 526 by radiation, convection current and/or conduction with heat transferred.By be arranged in the opening 514 independent pipeline or by the hole 543 in covering layer sleeve pipe 541, can remove oxidation product.Encapsulant 542 and strengthening material 544 can form described herein such.
Fig. 5 shows an embodiment of the device that is configured to heat the stratum of containing hydrocarbon.Electric heater 510 can be arranged in the opening 514 on the stratum 516 of containing hydrocarbon.Opening 514 can penetrate covering layer 540 and enter stratum 516 and form.Opening 514 can have at least approximately diameter of 5cm.As an example, opening 514 can have the diameter of about 13cm.Electric heater 510 can be heated at least a portion 518 that contains the stratum 516 of hydrocarbon the temperature (for example about 260 ℃) that is enough to support oxidation.This part 518 can have the width of about 1m.Can oxidation fluid (for example liquid or gas) by pipeline 512 or arbitrarily other suitable device for transferring fluid be fed in the opening.Pipeline 512 can have the critical flow orifice 515 of arranging along its length.Can such this critical flow orifice 515 that forms as described herein.
For example, pipeline 512 can be a conduit or pipe, and it is constructed to be permeable to oxidation fluid is fed in the opening 514 from oxidation fluid source 508.For example, pipeline 512 can be a stainless steel tube.Oxidation fluid can comprise that air or any other contain the fluid of oxygen (for example hydrogen peroxide, nitrogen oxide, ozone).Can use the mixture of oxidation fluid.The oxidation fluid mixture can comprise: the fluid that for example comprises 50 percent oxygen and 50 percent nitrogen.In certain embodiments, oxidation fluid also can comprise when according to the compound that discharges oxygen when heating like that described herein, for example hydrogen peroxide.This oxidation fluid can at least a portion hydrocarbon of oxidation in the stratum.
In certain embodiments, the heat interchanger that is arranged in stratum outside can be constructed to be permeable to heat this oxidation fluid.Heated oxidation fluid can be fed in the opening from this heat interchanger (directly or indirectly).For example, by being arranged in this opening and being fed in the opening from heat interchanger with oxidation fluid that pipeline that heat interchanger combines will be heated.In certain embodiments, pipeline can be a stainless steel tube.The oxidation fluid that heated is formed at least a portion on stratum heating or to have at least and help be heated to the temperature that is enough to support the hydrocarbon oxidation.After this is heated the temperature that partly reaches such, can reduce or stop at the heating of the oxidation fluid in the heat interchanger.
Fig. 6 shows another embodiment of the device that is constructed to be permeable to heat the stratum of containing hydrocarbon.Heat interchanger 520 can be arranged in the outside of the opening 514 in the stratum 516 of containing hydrocarbon.Can penetrate covering layer 540 and enter stratum 516 formation openings 514.Heat interchanger 520 can be supplied with heat from another surface process, and perhaps it can comprise heater (for example electric heater or burning heater).Oxidation fluid source 508 can be supplied with heat interchanger 520 to oxidation fluid.Heat interchanger 520 can the heated oxide fluid (for example more than 200 ℃ or reach the temperature that is enough to support the hydrocarbon oxidation).The oxidation fluid of this heating can be fed in the opening 514 by pipeline 521.Pipeline 521 can have the critical flow orifice 515 of arranging along its length.Can such critical flow orifice 515 that forms as described herein.The oxidation fluid of heating can or have at least the heating of at least a portion 518 on stratum and helps be heated to the temperature that is enough to support the hydrocarbon oxidation.This oxidation fluid can oxidation a part of hydrocarbon in the stratum at least.
In another embodiment, fuel fluid can be oxidized at the heater that is arranged in the outside, stratum of containing hydrocarbon.Can come oxidized fuel fluid with the oxidation fluid in the heater.As an example, this heater can be the heater of flame ignition.The fluid that fuel fluid can comprise arbitrarily and oxygen reacts.The example of fuel fluid can be methane, ethane, propane or other hydrocarbon or hydrogen and forming gas arbitrarily.Can supply with opening to the fuel fluid of oxidation from heater through piping, and turn back to ground through another pipeline in covering layer.This pipeline can be combined in the covering layer.In certain embodiments, can arrange these pipelines with one heart.The fuel fluid of oxidation is formed the heating of at least a portion on stratum or to have at least and help be heated to the temperature that is enough to support the hydrocarbon oxidation.When reaching such temperature, can replace the fuel fluid of oxidation with oxidation fluid.This oxidation fluid can the reaction zone of oxidation in the stratum at least a portion hydrocarbon.
Claims (13)
Applications Claiming Priority (2)
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| EPPCT/EP01/04641 | 2001-04-24 | ||
| PCT/EP2001/004641 WO2001081715A2 (en) | 2000-04-24 | 2001-04-24 | Method and system for treating a hydrocarbon containing formation |
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| CN01823289.2A Expired - Fee Related CN1271312C (en) | 2001-04-24 | 2001-10-11 | Electrical well heating system and method |
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| CN01823289.2A Expired - Fee Related CN1271312C (en) | 2001-04-24 | 2001-10-11 | Electrical well heating system and method |
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| CN102369339A (en) * | 2008-10-02 | 2012-03-07 | 美国页岩油公司 | Carbon sequestration in depleted oil shale deposits |
| CN102425399A (en) * | 2011-12-29 | 2012-04-25 | 新奥气化采煤有限公司 | oil shale mining method |
| CN101918761B (en) * | 2007-07-20 | 2012-06-27 | 国际壳牌研究有限公司 | flameless combustion heater |
| CN103917744A (en) * | 2011-10-24 | 2014-07-09 | 尼克森能源无限责任公司 | Vapor flooding with oxygen, and periodic steam stimulation with oxygen |
| CN105840162A (en) * | 2016-05-17 | 2016-08-10 | 赵金岷 | Underground combustion convection heating method |
| CN102369339B (en) * | 2008-10-02 | 2016-11-30 | 美国页岩油公司 | Carbon chelating in exhausted oil shale deposit thing |
| CN109339755A (en) * | 2018-12-03 | 2019-02-15 | 中国石油大学(北京) | A method and device for improving oil recovery of tight rock reservoirs |
| CN113286968A (en) * | 2018-11-12 | 2021-08-20 | Ws热加工技术有限责任公司 | Method and device for flameless staged combustion |
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| CN101316984A (en) * | 2005-10-24 | 2008-12-03 | 国际壳牌研究有限公司 | System and method for producing hydrocarbons from tar sands using heat-generated drainage channels |
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| RU2388790C1 (en) * | 2008-09-18 | 2010-05-10 | Открытое акционерное общество "Газпром промгаз" (ОАО "Газпром промгаз") | Thermal processing method of deep-lying slate coals |
| CA2709241C (en) | 2009-07-17 | 2015-11-10 | Conocophillips Company | In situ combustion with multiple staged producers |
| CA2850741A1 (en) * | 2011-10-07 | 2013-04-11 | Manuel Alberto GONZALEZ | Thermal expansion accommodation for circulated fluid systems used to heat subsurface formations |
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- 2001-10-10 DE DE60116387T patent/DE60116387T2/en not_active Expired - Lifetime
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- 2001-10-11 WO PCT/EP2001/011819 patent/WO2002086284A1/en active IP Right Grant
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- 2001-10-11 NZ NZ528898A patent/NZ528898A/en not_active IP Right Cessation
- 2001-10-11 AU AU2002224779A patent/AU2002224779B2/en not_active Ceased
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101918761B (en) * | 2007-07-20 | 2012-06-27 | 国际壳牌研究有限公司 | flameless combustion heater |
| CN102369339A (en) * | 2008-10-02 | 2012-03-07 | 美国页岩油公司 | Carbon sequestration in depleted oil shale deposits |
| CN102369339B (en) * | 2008-10-02 | 2016-11-30 | 美国页岩油公司 | Carbon chelating in exhausted oil shale deposit thing |
| CN103917744A (en) * | 2011-10-24 | 2014-07-09 | 尼克森能源无限责任公司 | Vapor flooding with oxygen, and periodic steam stimulation with oxygen |
| CN102425399A (en) * | 2011-12-29 | 2012-04-25 | 新奥气化采煤有限公司 | oil shale mining method |
| CN105840162A (en) * | 2016-05-17 | 2016-08-10 | 赵金岷 | Underground combustion convection heating method |
| CN105840162B (en) * | 2016-05-17 | 2019-09-17 | 赵金岷 | Underground combustion Convective Heating method |
| CN113286968A (en) * | 2018-11-12 | 2021-08-20 | Ws热加工技术有限责任公司 | Method and device for flameless staged combustion |
| US12241626B2 (en) | 2018-11-12 | 2025-03-04 | WS-Wärmeprozeßtechnik GmbH | Method and device for flameless stepwise combustion |
| CN109339755A (en) * | 2018-12-03 | 2019-02-15 | 中国石油大学(北京) | A method and device for improving oil recovery of tight rock reservoirs |
| CN109339755B (en) * | 2018-12-03 | 2019-12-31 | 中国石油大学(北京) | A method and device for increasing the recovery rate of tight rock reservoirs |
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| CA2445455A1 (en) | 2002-10-31 |
| EA005650B1 (en) | 2005-04-28 |
| CN1507529A (en) | 2004-06-23 |
| CA2445455C (en) | 2010-02-23 |
| CN1271312C (en) | 2006-08-23 |
| DE60116388T2 (en) | 2006-08-17 |
| IL158426A0 (en) | 2004-05-12 |
| ZA200308048B (en) | 2004-07-08 |
| EA200301149A1 (en) | 2004-04-29 |
| AU2002224779B2 (en) | 2007-02-01 |
| MA26016A1 (en) | 2003-12-31 |
| DE60116387D1 (en) | 2006-02-02 |
| NZ528899A (en) | 2004-07-30 |
| IL158427A0 (en) | 2004-05-12 |
| MA26167A1 (en) | 2004-07-01 |
| DE60116387T2 (en) | 2006-08-17 |
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