EP1996889A1 - Plate heat exchanger, method for its production, and its use - Google Patents
Plate heat exchanger, method for its production, and its useInfo
- Publication number
- EP1996889A1 EP1996889A1 EP07723516A EP07723516A EP1996889A1 EP 1996889 A1 EP1996889 A1 EP 1996889A1 EP 07723516 A EP07723516 A EP 07723516A EP 07723516 A EP07723516 A EP 07723516A EP 1996889 A1 EP1996889 A1 EP 1996889A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- heat exchanger
- plates
- plate heat
- exchanger according
- plate
- 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.)
- Granted
Links
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D9/00—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
- F28D9/0031—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other
- F28D9/0043—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other the plates having openings therein for circulation of at least one heat-exchange medium from one conduit to another
- F28D9/005—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other the plates having openings therein for circulation of at least one heat-exchange medium from one conduit to another the plates having openings therein for both heat-exchange media
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F13/00—Arrangements for modifying heat-transfer, e.g. increasing, decreasing
- F28F13/06—Arrangements for modifying heat-transfer, e.g. increasing, decreasing by affecting the pattern of flow of the heat-exchange media
- F28F13/12—Arrangements for modifying heat-transfer, e.g. increasing, decreasing by affecting the pattern of flow of the heat-exchange media by creating turbulence, e.g. by stirring, by increasing the force of circulation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/04—Constructions of heat-exchange apparatus characterised by the selection of particular materials of ceramic; of concrete; of natural stone
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F3/00—Plate-like or laminated elements; Assemblies of plate-like or laminated elements
- F28F3/02—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations
- F28F3/04—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element
- F28F3/048—Elements or assemblies thereof with means for increasing heat-transfer area, e.g. with fins, with recesses, with corrugations the means being integral with the element in the form of ribs integral with the element or local variations in thickness of the element, e.g. grooves, microchannels
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F2250/00—Arrangements for modifying the flow of the heat exchange media, e.g. flow guiding means; Particular flow patterns
- F28F2250/04—Communication passages between channels
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F2250/00—Arrangements for modifying the flow of the heat exchange media, e.g. flow guiding means; Particular flow patterns
- F28F2250/10—Particular pattern of flow of the heat exchange media
- F28F2250/102—Particular pattern of flow of the heat exchange media with change of flow direction
Definitions
- the invention relates to a plate heat exchanger of a plurality of plates, preferably made of sintered ceramic material, a method for producing such a plate heat exchanger and the use of such a plate heat exchanger as a high temperature heat exchanger and / or for use with corrosive media, as well as a reactor.
- Heat exchangers are particularly effective heat transfer between two separately flowing media, that is they should transfer as much heat as possible with as little exchange surface. At the same time they should oppose the material flows only a small resistance, so that the least possible energy has to be expended for the operation of the pumps used for promotion. If highly aggressive or corrosive media, possibly even at elevated temperatures of more than 200 ° C are passed through the heat exchanger, all materials in contact with the medium in the heat exchanger must be sufficiently resistant to corrosion. In addition to the replacement surfaces, this includes all seals and bushings. In addition, the design of heat exchangers should be designed so that, if necessary, a residue-free emptying of the heat exchanger is easily possible, for example, for maintenance.
- Plate heat exchangers are a special design of heat exchangers. They are characterized by a particularly compact design.
- the plates of a plate heat exchanger generally have an embossed or corrugated structure, often also called herringbone pattern or chevron pattern, in the region of the exchange surface.
- the embossing causes the medium flowing in the gap between two adjacent plates to become highly entangled, thereby promoting heat transfer.
- the medium is opposed by such a structure, a relatively low flow resistance.
- An effective heat transfer with the lowest possible pressure loss is so largely met.
- the plates are usually at the edges loosely on each other and are separated by seals. Since plastic seals can only be used up to temperatures of 300 ° C maximum, heat exchangers with plates made of metallic materials for higher operating temperatures or pressures solder or weld the plates together at the edges.
- the gap between two adjacent plates each forms a sealed chamber.
- a large chamber volume is both useful and therefore to strive for.
- an operating risk is also accepted. If no support segments are used in the chambers, it can easily lead to a plate break in the construction of an unforeseen high differential pressure between adjacent chambers to a strong deformation of the metal plates or in the case of brittle materials.
- Heat exchanger plates of this form are made of metallic materials, in particular corrosion-resistant steels, titanium or tantalum. Graphite is also used commercially.
- Sintered SiC ceramic is a universally corrosion-resistant but brittle material that is free of metallic silicon, in contrast to silicon-infiltrated silicon carbide (SiSiC).
- SiSiC silicon-infiltrated silicon carbide
- SSiC is ideally suited as a material for the exchange surface of heat exchangers due to its very high thermal conductivity.
- SSiC can also be used at high temperatures of well over 1,000 ° C.
- SSiC is also corrosion-resistant in hot water or strongly basic media.
- SSiC sintered SiC ceramics
- DE 197 17 931 C1 describes a fiber-reinforced ceramic (C / SiC or SiC / SiC) for use in heat exchangers at high temperatures of 200-1600 0 C and / or corrosive media. Compared to SSiC, these materials are significantly more costly and expensive to manufacture. In addition, the ceramic fiber composites C / SiC and SiC / SiC generally have a continuous porosity, whereby a hermetic tightness is not given. Even with an additional, complex and very expensive surface impregnation these disadvantages can not be overcome.
- EP 1 544 565 A2 describes the use of fiber-reinforced ceramic or of SiC especially for the plates of a high-temperature plate heat exchanger.
- the channel structure of the platform described therein Th has fins or ribs and is designed specifically for the flow of hot gases, especially for gas turbines. When using this construction for liquid media, the efficiency would not be good and the pressure loss too high.
- the plate heat exchanger continues to be produced by foil casting and joined by soldering. However, solder joints are always weak points when used with corrosive media, so that such a heat exchanger for use with highly corrosive media, such as alkalis, is not suitable.
- EP 0 074 471 B1 describes a production process for a ceramic plate heat exchanger by means of film casting and lamination.
- the laminating process is specially designed for SiSiC as a material and liquid siliconizing during production.
- FIG. 2 of this patent shows an embodiment of a gas heating heat exchanger in which baffles are provided perpendicular to the direction of flow, which are intended to effect a uniform temperature distribution in the flow channels.
- baffles are provided perpendicular to the direction of flow, which are intended to effect a uniform temperature distribution in the flow channels.
- the heat transfer performance and the pressure loss in this heat exchanger are not yet satisfactory.
- the invention is therefore based on the object to provide a plate heat exchanger with improved heat transfer performance and reduced pressure loss, which is also suitable for use at high temperatures and / or with corrosive media if necessary. Furthermore, a method for producing such a heat exchanger is to be specified.
- the above object is achieved by a plate heat exchanger of a plurality of plates according to claim 1, a method for producing such a plate heat exchanger according to claims 19 and 20, and the use of the plate heat exchanger according to claims 22 and 23.
- Advantageous or particularly expedient Ausgestaltun- conditions of the subject of the application are specified in the subclaims.
- the invention is thus a plate heat exchanger of a
- the invention further provides a method for producing such a plate heat exchanger, wherein the individual plates are stacked and each connected to each other by means of circumferential seals.
- the invention also relates to a method for producing such a plate heat exchanger, wherein the individual plates are stacked and joined in a diffusion welding process in the presence of a protective gas atmosphere or in a vacuum at a temperature of at least 1,600 ° C and optionally with application of a load to form a seamless monolithic block ,
- the plate heat exchanger according to the invention is suitable as a high-temperature heat exchanger and / or for use with corrosive media.
- the plate heat exchanger according to the invention can also be used as a reactor with at least two separate fluid circuits.
- the plate heat exchanger according to the invention is suitable as a reactor, wherein in addition one or more reactor plates are provided between the plates, wherein the reactor plates have a different channel system from the plates.
- the fluid flow guide channels are formed as a channel system so that a substantially meandering course of the fluid flow over the surface of the plate results, the side walls of the guide channels having a plurality of interruptions or openings, leading to a Turbulence of the fluid flow lead.
- brittle materials such as graphite or glass, preferably of sintered ceramic materials, in particular of SSiC.
- a further advantage of the design of the plates according to the invention is that feed and discharge openings for the fluid streams, for example in the form of bores, can already be integrated into the plates.
- the heat transfer in a plate heat exchanger according to the invention is compared to plate heat exchangers of the prior art by about 5 to 30% higher and the pressure loss is up to 30% lower.
- the pressure loss is an important criterion in the design of heat exchangers, because thus the required pump power can be reduced accordingly.
- the plate heat exchanger according to the invention has a structure in which a plurality of plates, preferably of sintered ceramic material, are stacked on each other.
- Sintered silicon carbide (SSiC), fiber-reinforced silicon carbide, silicon nitride or combinations thereof are particularly suitable as sintered ceramic material, with SSiC being particularly preferred.
- the sintered silicon carbide having a bimodal grain size distribution comprises 50 to 90% by volume of prismatic, platelet-shaped SiC crystallites having a length of 100 to 1,500 ⁇ m and 10 to 50% by volume of prismatic, platelet-shaped SiC crystallites of 5 to less than 5 100 ⁇ m.
- the measurement of the grain size or the length of the SiC crystallites can be carried out on the basis of light microscope micrographs, For example, with the aid of a Schmauslusprogramms, which determines the maximum Feret's diameter of a grain determined.
- the guide channels in the plates are connected to a first feed opening and a first discharge opening for a first fluid. Furthermore, a second supply opening and a second discharge opening for a second fluid for supplying an adjacent plate may be provided, these openings may be provided in a simple manner by drilling.
- a plate of a first plate type comprises a channel system for a first fluid and an adjacent plate of a second plate type a channel system for a second fluid.
- the first-disk-type disks and the second-disk-type disks may be sequenced in any order to allow for variable speed adjustment.
- the plates connected in parallel or in series are doubled or tripled by one of the two circuits of the heat exchanger in order to allow the material flow to be passed through the plates at a defined speed. This results in stacking sequences of the heat exchanger plates, for example, according to A-BB-A-BB ... or A-BBB-A-BBB ...
- the inventive design of the heat exchanger plates but also allows a so-called two or more common driving style.
- the plates of a circuit instead of parallel connected in series. This is the medium flowing through a longer distance for heating or cooling available.
- the channel system of the plates has a mirror symmetry.
- This mirror-symmetric design allows plates to be alternately stacked 180 ° apart, so that the feed openings are alternately left and right.
- By this arrangement can be constructed with a single design for all plates a heat exchanger, which offers advantages from a production point of view.
- within a plate at least two separate channel systems may be provided for different fluids between which heat transfer is to take place. In this case, it is preferred that the different fluids are guided in counterflow in separate channel systems.
- the plates used according to the invention preferably have a base thickness in the range of 0.2 to 20 mm, particularly preferably about 3 mm.
- the fluid or material flow in an exchange surface of a plate is guided in a meandering manner according to the channel system according to the invention in order to allow the longest possible residence time.
- the side walls or guide walls of the guide channels in the exchange surface have, measured from the plate base, preferably a height in the range of 0.2-30 mm, more preferably 0.2-10 mm, and particularly preferably 0.2-5 mm.
- the side walls of the guide channels designed as webs can be produced by means of milling, but they can also be manufactured by means of near net shape pressing.
- the side walls of the guide channels have at defined locations interruptions or openings, which preferably have a width of 0.2-20 mm, more preferably 2-5 mm.
- These breakthroughs cause a high turbulence of the fluid flow and, with the substantially meander-shaped flow course, permit a high and improved heat transfer efficiency.
- these breakthroughs allow a significant reduction in the conventional plate heat exchangers high pressure loss. Due to the number and width of the apertures, the pressure loss can be set in the desired manner. The breakthroughs also serve to ensure that the heat exchanger can be completely emptied when installed vertically.
- the perforated side walls of the guide channels also act as support points and avoid pressure differences in an undesirable deformation of the plates and also prevent a plate breakage.
- the individual plates are stacked and connected by means of peripheral seals.
- peripheral seals For this purpose, customary plastic seals, which can be used up to temperatures of about 300 0 C are suitable.
- the construction connected by seals is very cost-effective and then particularly advantageous. if the heat exchanger has to be disassembled and cleaned for inspection purposes.
- the individual plates are stacked and joined together to form an seamless monolithic block.
- This monolithic construction in which the panels are sealed without seams by seam-free joining, is particularly advantageous for applications at high temperatures and applications involving environmentally hazardous or corrosive media.
- the plate heat exchanger according to the invention, at least two of the plates are stacked and joined together to form an seamless monolithic block and at least two such monolithic blocks are connected to each other by means of circumferential seals.
- This so-called semi-sealed embodiment may be particularly useful when using corrosive media in a material cycle and from the tendency to deposit formation media in the other material cycle.
- the plates for the corrosive medium according to the invention sintered together at least in pairs and stacked the monolithic plate blocks thus obtained by suitable plastic seals, for example made of elastomeric material, sealed.
- This type of plate heat exchanger can always be disassembled, for example, to clean the sealed chambers of the deposit formation.
- the individual plates are used for producing a monolithic block as described above are stacked and, in a diffusion welding process in the presence of a protective gas atmosphere or under vacuum at a temperature of at least 1,600 ° C, preferably above 1,800 0 C, more preferably about 2,000 0 C and optionally under application of a Load joined to a seamless monolithic block, wherein the components to be joined preferably undergo a plastic deformation in the direction of force application of less than 5%, more preferably less than 1%.
- SSiC sintered SiC
- SSiC sintered SiC
- a bimodal as mentioned above Grain size distribution which may contain up to 35 vol .-% of other material components, such as graphite, boron carbide or other ceramic particles.
- the resistance to plastic deformation in the high temperature range is referred to in material science with high temperature creep resistance.
- the so-called creep rate is used.
- the creep rate of the ceramic plates to be joined can be used as a central parameter in order to minimize the plastic deformation in a joining process for seamless joining of the sintered ceramic plates.
- Most commercially available sintered SiC materials have structures with a monomodal particle size distribution and a particle size of about 5 ⁇ m. They thus have a sufficiently high sintering activity at joining temperatures of more than 1,700 ° C, but have low creep resistance for low-deformation joining. Therefore, hitherto, in the diffusion welding of such components, high plastic deformation has always been observed. Because the creep resistance of the SSiC materials is generally not very different, creep rate has not heretofore been considered as a useful variable parameter for SSiC joining.
- the creep rate of SSiC can be varied over a wide range by varying the structure formation. Only through the use of certain grades, such as those with bimodal particle size distribution, therefore, the low-deformation joining for SSiC materials is reached.
- the ceramic to be joined plates preferably consist of a SSiC material, the creep rate in the joining process is always less than 2 x 10 "4 l / s, is always preferably less than 8 x 10" 5 l / s, particularly preferably always lower than 2 x 10 "is 5 l / s.
- a load of more than 10 kPa, particularly preferably more than 1 MPa, and more preferably more than 10 MPa, is preferably applied, the temperature-holding time at a temperature of at least 1,600 ° C. preferably having a duration of 10 minutes, particularly preferably Exceeds 30 minutes.
- the plate heat exchanger thus produced from sintered SiC ceramic therefore have an extremely high temperature and corrosion resistance.
- the plate heat exchanger with heat exchanger plates designed according to the invention is also suitable as a reactor, for example for evaporation and condensation, but also for other phase transformations, such as, for example, for targeted crystallization processes.
- a reactor for example for evaporation and condensation, but also for other phase transformations, such as, for example, for targeted crystallization processes.
- reactor plates For a particularly effective use as a reactor, it is expedient to see between the inventively designed heat exchanger plates install reactor plates, in which case the heat exchanger plates are used for temperature control of the reactor plates.
- the reactor plates can have different geometries.
- For a controlled residence time and defined precipitation reaction, such as for targeted crystallization processes it is for example advantageous to use reactor plates with continuous straight channels.
- channel structures are used with which the material flows are supplied to one another in a defined region of the reactor plate and mixed intensively.
- the reactor plates may also have suitable catalytic coatings that specifically accelerate a chemical reaction.
- the plate heat exchanger further comprises a ceramic or metallic Anflanschsystem for the supply and discharge of fluids on the top and / or bottom (lid and / or bottom) of the plate heat exchanger.
- a mica-based sealing material for the sealing of the Flange system is preferably used for high-temperature applications.
- FIG. 1 shows the plan view of a sintered ceramic material heat exchanger plate used in accordance with the invention
- Figure 2 shows the top view of a reactor plate used in the invention.
- Figures 3a and 3b are photographs of plate heat exchangers according to the invention, including flanging systems.
- a plate 1 which can be used according to the invention has a channel system formed by guide channels 2, which allows a substantially meandering course of the fluid flow over the surface of the plate.
- the side walls 3 of the guide channels 2 consist in this figure of webs with a width of 3 mm, which have a plurality of apertures 4 with a width of 3.5 mm.
- the plate further has a first feed opening 5 and a first discharge opening 6 for a fluid flow, each in the form of a bore with a radius of 30 mm.
- a second feed opening 7 and a second discharge opening 8, which serve as a passage for supplying a neighboring chamber with another medium, are provided.
- the second feed opening and second discharge opening each consist of holes with a radius of 32 mm.
- the total length of the plate in this embodiment is 500 mm and its width is 200 mm.
- the channel system in this embodiment has a mirror symmetry. This mirror symmetry makes it possible for the plates to be alternately stacked against each other rotated through 180 °, so that the feed openings are alternately once on the left and once on the right.
- FIG. 2 shows a reactor plate 9 which can be used according to the invention with a first feed opening 10 for a first fluid flow and a second feed flow Feed opening 1 1 for a second fluid flow.
- the two fluid streams are then supplied to each other through the baffles 12 so that an intensive mixing of the Fiuidströme takes place.
- the mixed stream is then removed via the discharge opening 13.
- Figures 3a and 3b show how metallic flanges are clamped to a ceramic monolith.
- a ceramic heat exchanger is manufactured with heat exchanger plates in the manner of Figure 1.
- the plates have a length of 500 mm, a bottom thickness of 3 mm and guide channels with a height of 3.5 mm.
- the side walls have openings of a width of 3 mm.
- For the production of the heat exchanger block four heat exchanger plates according to the invention and a cover plate are used, wherein all components consist of sintered silicon carbide with bimodal particle size distribution. All ceramic panels are stacked and bonded together to form a monolithic block.
- the plates are arranged in the block so that two streams can exchange heat in countercurrent.
- the hermetically sealed sintered silicon carbide heat exchanger block is provided with four 50mm internal diameter flanges.
- the heat exchanger apparatus is operated with aqueous media. At a flow rate of 1000 l / h, a pressure drop of 100 mbar occurs and 6000 W / m 2 K are transferred.
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Heat-Exchange Devices With Radiators And Conduit Assemblies (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
- Details Of Heat-Exchange And Heat-Transfer (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102006013503A DE102006013503A1 (en) | 2006-03-23 | 2006-03-23 | Plate heat exchanger, process for its preparation and its use |
PCT/EP2007/002565 WO2007110196A1 (en) | 2006-03-23 | 2007-03-22 | Plate heat exchanger, method for its production, and its use |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1996889A1 true EP1996889A1 (en) | 2008-12-03 |
EP1996889B1 EP1996889B1 (en) | 2011-11-30 |
Family
ID=38267705
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP07723516A Not-in-force EP1996889B1 (en) | 2006-03-23 | 2007-03-22 | Plate heat exchanger, method for its production, and its use |
Country Status (9)
Country | Link |
---|---|
US (1) | US8967238B2 (en) |
EP (1) | EP1996889B1 (en) |
JP (1) | JP2009530582A (en) |
CN (1) | CN101405554B (en) |
AT (1) | ATE535769T1 (en) |
CA (1) | CA2643757C (en) |
DE (1) | DE102006013503A1 (en) |
ES (1) | ES2373992T3 (en) |
WO (1) | WO2007110196A1 (en) |
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2006
- 2006-03-23 DE DE102006013503A patent/DE102006013503A1/en not_active Withdrawn
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2007
- 2007-03-22 JP JP2009500779A patent/JP2009530582A/en active Pending
- 2007-03-22 EP EP07723516A patent/EP1996889B1/en not_active Not-in-force
- 2007-03-22 WO PCT/EP2007/002565 patent/WO2007110196A1/en active Application Filing
- 2007-03-22 AT AT07723516T patent/ATE535769T1/en active
- 2007-03-22 CA CA2643757A patent/CA2643757C/en not_active Expired - Fee Related
- 2007-03-22 CN CN2007800103720A patent/CN101405554B/en not_active Expired - Fee Related
- 2007-03-22 ES ES07723516T patent/ES2373992T3/en active Active
- 2007-03-22 US US12/225,425 patent/US8967238B2/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
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See references of WO2007110196A1 * |
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US20090151917A1 (en) | 2009-06-18 |
US8967238B2 (en) | 2015-03-03 |
CN101405554A (en) | 2009-04-08 |
CA2643757A1 (en) | 2007-10-04 |
ATE535769T1 (en) | 2011-12-15 |
CN101405554B (en) | 2011-05-11 |
WO2007110196A1 (en) | 2007-10-04 |
EP1996889B1 (en) | 2011-11-30 |
JP2009530582A (en) | 2009-08-27 |
ES2373992T3 (en) | 2012-02-10 |
CA2643757C (en) | 2011-09-27 |
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