EP2212637B1 - Method for mechanical dehydration with thermal assistance - Google Patents

Method for mechanical dehydration with thermal assistance Download PDF

Info

Publication number
EP2212637B1
EP2212637B1 EP08871924.0A EP08871924A EP2212637B1 EP 2212637 B1 EP2212637 B1 EP 2212637B1 EP 08871924 A EP08871924 A EP 08871924A EP 2212637 B1 EP2212637 B1 EP 2212637B1
Authority
EP
European Patent Office
Prior art keywords
temperature
pressure
liquid
heated
wall
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.)
Not-in-force
Application number
EP08871924.0A
Other languages
German (de)
French (fr)
Other versions
EP2212637A2 (en
Inventor
Maria Aurora Fernandez
Bernard Auduc
Patricia Arlabosse
Akrama Mahmoud
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.)
Ecole Nationale Superieure Des Mines D'albi-Carmau
Original Assignee
ECOLE NATIONALE SUPERIEURE DES MINES D'ALBI-CARMAUX
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 ECOLE NATIONALE SUPERIEURE DES MINES D'ALBI-CARMAUX filed Critical ECOLE NATIONALE SUPERIEURE DES MINES D'ALBI-CARMAUX
Publication of EP2212637A2 publication Critical patent/EP2212637A2/en
Application granted granted Critical
Publication of EP2212637B1 publication Critical patent/EP2212637B1/en
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B7/00Drying solid materials or objects by processes using a combination of processes not covered by a single one of groups F26B3/00 and F26B5/00

Definitions

  • the present invention relates to a method of thermally assisted mechanical dehydration for the purpose of achieving the solid / liquid separation of a product comprising on the one hand a liquid phase and on the other hand a solid phase.
  • the separation of a continuous phase (the liquid) and a dispersed phase (the solid) initially mixed can be carried out in various ways: decantation, centrifugation, filtration, compression, magnetic separation, ....
  • decantation centrifugation
  • filtration filtration
  • compression filtration
  • magnetic separation rotary separation
  • One of the techniques of dehydration mechanically conventionally implemented in the industry is the series coupling of a constant pressure filtration and a mechanical compression.
  • the filtration is applied to suspensions, concentrated or diluted, of coarse particles possibly having a spread particle size distribution as well as colloidal suspensions.
  • the separation is carried out using a filter medium permeable essentially to the liquid phase of the mixture to be separated.
  • the separated liquid is called the filtrate, the effluent or the permeate.
  • a suspension to be filtered is introduced at a constant rate or, more frequently, under constant supply pressure in a closed chamber by a porous support (the filter media).
  • the suspension migrates to the filter medium, on which the solid particles are deposited and form a filter cake while the filtrate is recovered under the porous support.
  • phase separation is never complete: the cake has residual moisture and the filtrate often contains some solids.
  • the separation can be continued by compression. The increase in pressure reduces the volume of the cake by expelling the excess liquid contained in the pores, which leads to a decrease in the residual moisture of the cake. For wet split solids, only the compression phase is implemented.
  • the solid / liquid separation usually begins with a step of thickening the product followed by a mechanical dewatering step during which the liquid contained in the product is separated in liquid form without the addition of heat.
  • the liquid content usually water
  • the efficiency of the mechanical separation is, however, rather poor for colloidal suspensions or pasty products, such as residual sludge.
  • the main advantage of these operations is their low energy consumption. For gravity thickening, consumption between 0.001 and 0.01 kWh is required per cubic meter of water removed. In a mechanical dewatering operation, the energy consumption is of the order of 1 to 10 kWh per cubic meter of water removed.
  • thermal drying which consists of evaporating or vaporizing the water contained in the wet product, can be used.
  • the energy cost of this operation is here of the order of 1000 kWh per cubic meter of water eliminated.
  • the cost of this operation is often prohibitive especially when the operation is practiced on by-products or waste.
  • the final water content of the dried products is generally less than 5%, although such a low water content is not always essential for the recovery of the waste.
  • the pressures used are relatively high and heat gains are such that they allow vaporization of the liquid phase.
  • a thermally assisted mechanical dehydration process comprising the features of the preamble of claim 1 is known from the document US 4380496 .
  • the present invention therefore aims to provide a thermally assisted mechanical dehydration process having an optimized energy balance.
  • this method will make it possible to avoid the problems of sticking encountered with certain methods of the prior art.
  • the present invention provides a thermally assisted mechanical dehydration process in which a product to be dehydrated is introduced into a filtration device and / or compression and wherein a heat input is achieved.
  • this method comprises a first step at a first pressure of less than 7 bar during which the product to be dehydrated is heated to a temperature below the evaporation temperature of the liquid to be removed and the liquid to be removed is recovered. progressively, this first step having a duration of between 5 minutes and several hours.
  • the first pressure is between 1.5 and 4 bar, preferably around 3 bar for the majority of products for which the process has been tested.
  • the filtration and / or compression device comprises an enclosure having a wall of which at least a portion is heated, and that the product to be dehydrated is heated by conduction from the heated portion of the wall.
  • the portion of the wall of the enclosure that is heated may be fixed or movable. If the pressure is achieved by a piston, trays or other elements, it can be provided that the means for exerting pressure on the product to be dehydrated are heated. Heating can be achieved by any means: electrical resistance, heat transfer fluid, radiation etc.
  • the method according to the invention provides that the first low pressure step is followed by a second step at a second pressure, this second pressure being greater than the first pressure and less than 30 bars.
  • This second pressure being greater than the first pressure and less than 30 bars.
  • An additional separation is thus achieved which makes it possible to increase the efficiency of the process.
  • this increase in yield is noticeable but it has been noticed with some other products that this second step at higher pressure could extract relatively little liquid.
  • the temperature preferably remains lower than the vaporization temperature of the liquid to be extracted.
  • the heated portion of the wall remains at a substantially constant temperature, this temperature corresponding to the temperature of said heated portion of the wall in the filtration and / or compression device at the end of the first step.
  • the heated portion of the wall preferably remains at a substantially constant temperature, this temperature corresponding to the temperature of said heated portion of the wall in the filtering device and / or compression at the end of the first compression step.
  • the heated portion of the wall is brought to a temperature of, for example, between 40 Ā° C. and 90 Ā° C. in the first step.
  • the method according to the invention may also comprise, before the first step, a dehydration step at room temperature, without the addition of heat, at a pressure corresponding to the first pressure.
  • the process according to the invention makes it possible to obtain higher yields with a lower energy consumption when it is applied, for example, to the pretreatment of a wet biomass, excluding wood.
  • the wet biomass treated here can be, for example, cereals, forage plants, leguminous plants, fiber plants, oleaginous plants, dye plants, etc. Among these plants, it is for example possible to mention non-limiting examples include alfalfa, ryegrass, soybean and pastel.
  • this wet biomass after thermally assisted mechanical dehydration, may for example undergo a final step of thermal drying in a dryer, the dryer then being advantageously equipped with a heat exchanger heat output, and the fog energy recovered in the heat exchanger being at least partially used to achieve heating in the previous steps of the method. In this way, it is possible to optimize the energy balance of the entire treatment chain of the biomass used in the process.
  • a method according to the invention can also be applied for example to the dehydration of liquid or pasty waste, excluding urban waste sludge and drinking water sludge.
  • This may be industrial sludge such as for example paper sludge or even a waste such as sodium bentonite used.
  • a method according to the invention is also well suited to the extraction of green juice from a wet biomass, excluding wood. This is for example to extract a high protein juice from a plant such as alfalfa. The liquid discharged during the dehydration is then recovered and is not a waste. To promote in this process the quality of green juice from thermally assisted mechanical dehydration, the temperature of the heated wall advantageously remains below 60 Ā° C. Preferably, the temperature of the heated walls is of the order of 50 Ā° C (+/- 2 Ā° C).
  • the figure 1 represents a filtration / compression cell that can be used for carrying out a method according to the invention.
  • This cell comprises firstly a cylinder 2 for receiving a product to be dewatered and secondly a piston 4 adapted to the cylinder 2 so as to slide therein.
  • the cylinder 2 is for example machined in polytetrafluoroethylene, known under the brand Teflon and which is a thermal insulating material.
  • the piston 4 can be made of copper, for example. Electrical resistors 6 are integrated in the piston 4 so as to heat it.
  • An outer casing 8 for example made of steel, provides the mechanical strength of the assembly.
  • a filter medium 10 which comprises firstly a glass microfiber filter deposited on a grid made for example of a teflon brand material. It is noted under the filter media the presence of a collector 12 of liquid. An outlet 14 is provided for the evacuation of the liquid collected at the collector 12.
  • a filtration / compression cell such as that shown on the figure 1 is intended to be inserted in a hydraulic press (not shown), for example a Carver hydraulic press.
  • the product to be dehydrated is poured into the cylinder 2 of the filtration / compression cell.
  • the piston 4 is then introduced into the cylinder 2 and compresses the product to be dehydrated.
  • a constant pressure is then exerted by this piston 4 on the product to be dehydrated in the cylinder 2.
  • a filtrate flows through the filter medium 10 to the collector 12 and is discharged through the outlet 14.
  • the first phase can be subdivided into two sub-phases: all firstly a first sub-phase where the product to be dehydrated is pressurized at ambient temperature and a second sub-phase where the piston rises in temperature until reaching the temperature T.
  • the process according to the invention has been applied as non-limiting examples to bentonite, alfalfa and paper mills.
  • the pressure P1 was chosen at 3 bar while, for the paper sludge, the pressure P1 is 1.78 bar.
  • the pressure P2 during the second phase is chosen to be greater than the pressure P1 while remaining less than 30 bars.
  • the Figures 2 and 3 show the results obtained with bentonite.
  • This mineral material is used in the field of civil engineering to fix soil and embankments during construction. It is a clay that has been treated to give it special plastic properties.
  • the bentonite is recovered and reused as long as its rheological properties are not altered.
  • the product is stored. It is noted that the bentonite thus stored contains about 90% water. It is therefore interesting to dehydrate this bentonite on the one hand to limit its mass during transport and on the other hand to limit its volume.
  • the figure 2 illustrates the mass percentage of water removed during the first phase, as a function of the temperature of the piston 4.
  • the duration of this first phase is set here to 3 hours. As well as the other numerical values indicated, this value is given for illustrative and not limiting. With such a duration, a temperature gradient is established in the product to be dehydrated in the filtration / compression cell.
  • the heating of the product to be dehydrated is carried out here by conduction.
  • Other heating modes can be envisaged. In particular, it is possible to heat the product before introducing it into the filtration / compression cell. This solution is not preferred because it requires heating water (or other liquid) which is then removed - hot - during the pressurization of the product to be dehydrated in the filtration / compression cell.
  • the mass percentage of water removed is calculated in the same way next: it is the ratio between the mass of water separated during a phase of the process and the total mass of water in the material. This ratio is always less than 1 and is expressed as a percentage in the figures.
  • the figure 2 represents the mass percentage of water removed after 3 hours for different temperatures of the piston 4.
  • the temperature T of the piston varies here between 21 Ā° C and 90 Ā° C. It is found that the amount of water removed increases with the temperature of the piston. For temperatures of the order of 80 to 90 Ā° C, it is noted that 70% of the water contained in the bentonite is removed. Depending on the needs of the user, this mass reduction of the bentonite may be sufficient.
  • the present invention can also be implemented with alfalfa.
  • industrial dewatering is an alternative to silage and dehydration in the field.
  • Dehydration allows the best preservation of the initial qualities of the forage. This process of transformation has developed strongly in France, which has become one of the leading producers of dehydrated fodder in Europe.
  • Dehydrated alfalfa production is currently in the range of 12 to 15 tonnes of dry matter per hectare per year. However, the current cost of energy strongly penalizes this mode of treatment.
  • alfalfa The dehydration of alfalfa is currently carried out by so-called ā€œdry processesā€, that is to say by implementing exclusively thermal drying and leading to the development of the meal in animal feed, or processes, called ā€œwetā€.
  • dry processes that is to say by implementing exclusively thermal drying and leading to the development of the meal in animal feed, or processes, called ā€œwetā€.
  • the latter implement a preliminary step of dehydration by screw press.
  • These "wetā€ processes make it possible to separate an aqueous phase (green juice), which is rich in proteins and natural pigments.
  • Such processes thus make it possible to obtain, on the one hand, the meal for animal feed and, on the other hand, to enhance the use of green juice in animal or human nutrition.
  • the process according to the invention makes it possible to increase the yield of the separation.
  • the duration of the first phase was fixed at 4 hours. That of the second phase was fixed at 2 hours.
  • Dryness is a parameter used to indicate the percentage by mass of dry matter contained in a product.
  • the dryness of a product is therefore the ratio between the dry mass contained in this product and the total mass of the product. Here too, it is a ratio of less than 1 which is expressed as a percentage. Dryness can also be considered as the ratio of the dry mass of the product to the sum of the dry mass and the water content of this product.
  • Alfalfa is assumed to have an initial dryness of 20%. Conventional pressing methods make it possible to obtain a dryness of 32.5%. After drying in a thermal dryer, the final dryness is about 87%.
  • the amount of liquid (green juice) separated by a route mechanical is 380 kg / h and the amount of water evaporated in the heat dryer to achieve a final dryness of 87% is 390 kg / h.
  • the amount of liquid (green juice) produced is 680 kg / h and the amount of water evaporated in the thermal dryer is 90 kg / h.
  • This (realistic) numerical example illustrates the gains that can be made for the dehydration of alfalfa.
  • the mass gain in green juice is more than 75% while the amount of water to be evaporated is approximately divided by four.
  • the temperature of the heated wall is preferably of the order of 50 Ā° C.
  • the figure 8 illustrates a dehydration pathway for alfalfa cake.
  • Two stages are represented here: a first stage of mechanical dehydration and a stage of thermal drying.
  • the dryness of the alfalfa is S initial
  • the two stages it is S intermediate and after the second stage, she is S final .
  • the energy supplied in the first step is X 1 , expressed in kWh per ton of separated water and that the energy supplied in the second step is X 2 , expressed in kWh per ton of separate water.
  • the power consumed on the conventional sector amounts to 312.25 kW for the sector incorporating the rotary kiln and 227.44 kW for the die integrating the pre-dryer upstream of the rotary kiln.
  • These results on the global sector can also be expressed in terms of specific consumption, which gives 405.45 kWh / t of water for the sector integrating the rotary kiln and 295.33 kWh / t of water for the integrated sector. the pre-dryer upstream of the rotary kiln.
  • the filter press is replaced by a device implementing a thermally assisted dehydration process as described for example above.
  • Energy consumption associated with this mechanical assisted mechanical separation was determined by the laboratory pilot described above. The values are shown in the following table for different piston wall temperatures. ā‡ b> Table 1 Energy consumption of assisted dehydration process ā‡ / b> Wall temperature (Ā° C) Energy consumption (kWh / t separate juice) 50 121.08 70 150.83
  • the figures 5 and 6 relate to the results obtained with stationary sludge using the process according to the invention. These figures correspond to Figures 2 and 3 described in application to bentonite.
  • the duration of the first phase is 30 minutes while the second phase lasts 15 minutes.
  • the figure 5 shows that, for stationary sludge, the influence of temperature is relatively low for the first phase. Indeed, while at 25 Ā° C the mass percentage of water removed is of the order of 66%, it is only about 67.5% at 80 Ā° C.
  • the second phase is interesting here because it allows to eliminate about 15 to 20% additional water.
  • the higher the pressure the more the quantity of separated water is also important.
  • P2 7.3 bars at 10.7 bars.
  • the interest of the thermally assisted mechanical dehydration process according to the invention is proven for the dehydration of bentonite and forage plants, such as alfalfa.
  • Applications in the agri-food field can be envisaged.
  • the method described above can be used for plants, especially woody plants, herbaceous legumes, tomatoes, beets, etc.
  • Agricultural by-products or green waste can also be treated with a method according to the invention. .
  • the present invention can be applied to any biomass but excludes the following definition of wood and sludge as well as drinking water sludge.
  • the present invention in this preferred embodiment, relies on two thermally assisted separation steps: a first stage, filtration or compression depending on the dehydrated material, at low pressure (of the order of 3 bar in a preferred embodiment) followed by a separation step at higher pressure, the piston temperature remains constant.
  • the first step makes it possible to separate a large quantity of liquid at a lower cost.
  • the second phase of separation a significant increase in dryness can be expected, depending on the dehydrated products, even at low pressure (of the order of 7 bars).
  • the separation is faster than at room temperature.
  • the technology of the screw press can be used in the present invention.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Processing Of Solid Wastes (AREA)
  • Treatment Of Sludge (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The method involves heating a product to be dehydrated at temperature lower than the temperature of evaporation of a liquid e.g. water, to be extracted, within a duration ranging between 5 minutes and hours when pressure is lower than 7 bars. The product is heated by conduction from a heated portion of a wall in a compression and/or filtration device. The heated portion of the wall is set to temperature ranging between 40 and 90 degree Celsius.

Description

La prƩsente invention concerne un procƩdƩ de dƩshydratation mƩcanique assistƩe thermiquement ayant pour but de rƩaliser la sƩparation solide/liquide d'un produit comportant d'une part une phase liquide et d'autre part une phase solide.The present invention relates to a method of thermally assisted mechanical dehydration for the purpose of achieving the solid / liquid separation of a product comprising on the one hand a liquid phase and on the other hand a solid phase.

La sĆ©paration d'une phase continue (le liquide) et d'une phase dispersĆ©e (le solide) initialement mĆ©langĆ©es peut ĆŖtre rĆ©alisĆ©e de diverses maniĆØres : dĆ©cantation, centrifugation, filtration, compression, sĆ©paration magnĆ©tique, .... Une des techniques de dĆ©shydratation mĆ©canique conventionnellement mise en oeuvre dans l'industrie est le couplage en sĆ©rie d'une filtration Ć  pression constante et d'une compression mĆ©canique.The separation of a continuous phase (the liquid) and a dispersed phase (the solid) initially mixed can be carried out in various ways: decantation, centrifugation, filtration, compression, magnetic separation, .... One of the techniques of dehydration mechanically conventionally implemented in the industry is the series coupling of a constant pressure filtration and a mechanical compression.

La filtration s'applique Ć  des suspensions, concentrĆ©es ou diluĆ©es, de particules grossiĆØres prĆ©sentant Ć©ventuellement une distribution granulomĆ©trique Ć©talĆ©e tout comme Ć  des suspensions colloĆÆdales. La sĆ©paration est rĆ©alisĆ©e Ć  l'aide d'un mĆ©dia filtrant permĆ©able essentiellement Ć  la phase liquide du mĆ©lange Ć  sĆ©parer. Le liquide sĆ©parĆ© s'appelle le filtrat, l'effluent, ou encore le permĆ©at.The filtration is applied to suspensions, concentrated or diluted, of coarse particles possibly having a spread particle size distribution as well as colloidal suspensions. The separation is carried out using a filter medium permeable essentially to the liquid phase of the mixture to be separated. The separated liquid is called the filtrate, the effluent or the permeate.

Dans le cas d'une filtration sur support, une suspension Ć  filtrer est introduite Ć  dĆ©bit constant ou, plus frĆ©quemment, sous pression d'alimentation constante dans une enceinte fermĆ©e par un support poreux (le mĆ©dia filtrant). Sous l'effet de la pression appliquĆ©e, la suspension migre vers le mĆ©dia filtrant, sur lequel les particules solides se dĆ©posent et forment un gĆ¢teau de filtration tandis que le filtrat est rĆ©cupĆ©rĆ© sous le support poreux. Comme dans d'autres procĆ©dĆ©s de sĆ©paration, la sĆ©paration des phases n'est jamais complĆØte : le gĆ¢teau prĆ©sente une humiditĆ© rĆ©siduelle et le filtrat contient souvent quelques solides. Lorsque les gĆ¢teaux de filtration formĆ©s sont compressibles, la sĆ©paration peut ĆŖtre poursuivie par compression. L'augmentation de pression rĆ©duit le volume du gĆ¢teau en expulsant le liquide en excĆØs contenu dans les pores, ce qui conduit Ć  une diminution de l'humiditĆ© rĆ©siduelle du gĆ¢teau. Pour des solides divisĆ©s humides, seule la phase de compression est mise en oeuvre.In the case of a supported filtration, a suspension to be filtered is introduced at a constant rate or, more frequently, under constant supply pressure in a closed chamber by a porous support (the filter media). Under the effect of the pressure applied, the suspension migrates to the filter medium, on which the solid particles are deposited and form a filter cake while the filtrate is recovered under the porous support. As in other separation processes, phase separation is never complete: the cake has residual moisture and the filtrate often contains some solids. When the formed filter cakes are compressible, the separation can be continued by compression. The increase in pressure reduces the volume of the cake by expelling the excess liquid contained in the pores, which leads to a decrease in the residual moisture of the cake. For wet split solids, only the compression phase is implemented.

Pour les suspensions, la sĆ©paration solide/liquide dĆ©bute habituellement par une Ć©tape d'Ć©paississement du produit suivie d'une Ć©tape de dĆ©shydratation mĆ©canique au cours de laquelle le liquide contenu dans le produit est sĆ©parĆ© sous forme liquide sans apport de chaleur. Lors de cette opĆ©ration, la teneur en liquide, en gĆ©nĆ©ral de l'eau, peut ĆŖtre rĆ©duite de 95 Ć  70% en masse. Ces chiffres sont variables selon les produits dĆ©shydratĆ©s et sont donnĆ©s ici Ć  titre purement indicatif. Le rendement de la sĆ©paration mĆ©canique est cependant assez mĆ©diocre pour les suspensions colloĆÆdales ou les produits pĆ¢teux, tels les boues rĆ©siduaires. L'atout principal de ces opĆ©rations est leur faible consommation Ć©nergĆ©tique. Pour un Ć©paississement gravitaire, une consommation comprise entre 0,001 et 0,01 kWh est nĆ©cessaire par mĆØtre cube d'eau Ć©liminĆ©. Dans une opĆ©ration de dĆ©shydratation mĆ©canique, la consommation d'Ć©nergie est de l'ordre de 1 Ć  10 kWh par mĆØtre cube d'eau Ć©liminĆ©.For suspensions, the solid / liquid separation usually begins with a step of thickening the product followed by a mechanical dewatering step during which the liquid contained in the product is separated in liquid form without the addition of heat. During this operation, the liquid content, usually water, can be reduced from 95 to 70% by weight. These figures are variable depending on the dehydrated products and are given here for information only. The efficiency of the mechanical separation is, however, rather poor for colloidal suspensions or pasty products, such as residual sludge. The main advantage of these operations is their low energy consumption. For gravity thickening, consumption between 0.001 and 0.01 kWh is required per cubic meter of water removed. In a mechanical dewatering operation, the energy consumption is of the order of 1 to 10 kWh per cubic meter of water removed.

Lorsqu'une rĆ©duction plus importante de la teneur en eau est nĆ©cessaire, le sĆ©chage thermique, qui consiste Ć  Ć©vaporer ou vaporiser l'eau contenue dans le produit humide, peut ĆŖtre utilisĆ©. Le coĆ»t Ć©nergĆ©tique de cette opĆ©ration est ici de l'ordre de 1000 kWh par mĆØtre cube d'eau Ć©liminĆ©. Le coĆ»t de cette opĆ©ration est souvent rĆ©dhibitoire surtout lorsque l'opĆ©ration est pratiquĆ©e sur des sous-produits ou des dĆ©chets. En outre, la teneur en eau finale des produits sĆ©chĆ©s est gĆ©nĆ©ralement infĆ©rieure Ć  5%, bien qu'une si basse teneur en eau ne soit pas toujours indispensable pour la valorisation du dĆ©chet.When a greater reduction in water content is required, thermal drying, which consists of evaporating or vaporizing the water contained in the wet product, can be used. The energy cost of this operation is here of the order of 1000 kWh per cubic meter of water eliminated. The cost of this operation is often prohibitive especially when the operation is practiced on by-products or waste. In addition, the final water content of the dried products is generally less than 5%, although such a low water content is not always essential for the recovery of the waste.

Il est connu de rĆ©aliser un apport de chaleur lors d'une dĆ©shydratation mĆ©canique. On parle alors de dĆ©shydratation mĆ©canique assistĆ©e thermiquement. Le couplage pression/chaleur peut s'envisager de diffĆ©rentes faƧons : d'une part selon le mode d'apport de cette chaleur (conduction, convection...) et d'autre part selon le moment oĆ¹ elle est apportĆ©e (avant l'Ć©tape de filtration, pendant la compression ou tout au long de la dĆ©shydratation).It is known to provide heat input during mechanical dewatering. This is known as thermally assisted mechanical dehydration. The pressure / heat coupling can be considered in different ways: on the one hand according to the mode of contribution of this heat (conduction, convection ...) and on the other hand according to the moment when it is brought (before the filtration stage, during compression or throughout dehydration).

Le plus souvent, les pressions utilisƩes sont relativement ƩlevƩes et les apports de chaleur sont tels qu'ils permettent une vaporisation de la phase liquide.Most often, the pressures used are relatively high and heat gains are such that they allow vaporization of the liquid phase.

Un procƩdƩ de dƩshydratation mƩcanique assistƩe thermiquement comprenant les caractƩristiques du prƩambule de la revendication 1 est connu du document US 4380496 .A thermally assisted mechanical dehydration process comprising the features of the preamble of claim 1 is known from the document US 4380496 .

Ces divers procƩdƩs prƩsentent tous l'inconvƩnient d'avoir un rendement ƩnergƩtique relativement mƩdiocre. En outre, on remarque parfois un collage du matƩriau sur les parois chaudes de la presse.These various methods all have the disadvantage of having a relatively poor energy efficiency. In addition, there is sometimes a sticking of the material on the hot walls of the press.

La prĆ©sente invention a alors pour but de fournir un procĆ©dĆ© de dĆ©shydratation mĆ©canique assistĆ© thermiquement prĆ©sentant un bilan Ć©nergĆ©tique optimisĆ©. De prĆ©fĆ©rence, ce procĆ©dĆ© permettra d'Ć©viter les problĆØmes de collage rencontrĆ©s avec certains procĆ©dĆ©s de l'art antĆ©rieur.The present invention therefore aims to provide a thermally assisted mechanical dehydration process having an optimized energy balance. Preferably, this method will make it possible to avoid the problems of sticking encountered with certain methods of the prior art.

ƀ cet effet, la prĆ©sente invention propose un procĆ©dĆ© de dĆ©shydratation mĆ©canique assistĆ©e thermiquement dans lequel un produit Ć  dĆ©shydrater est introduit dans un dispositif de filtration et/ou de compression et dans lequel un apport de chaleur est rĆ©alisĆ©.For this purpose, the present invention provides a thermally assisted mechanical dehydration process in which a product to be dehydrated is introduced into a filtration device and / or compression and wherein a heat input is achieved.

Selon la prĆ©sente invention, ce procĆ©dĆ© comporte une premiĆØre Ć©tape Ć  une premiĆØre pression infĆ©rieure Ć  7 bars au cours de laquelle le produit Ć  dĆ©shydrater est chauffĆ© Ć  une tempĆ©rature infĆ©rieure Ć  la tempĆ©rature d'Ć©vaporation du liquide Ć  Ć©liminer et le liquide Ć  Ć©liminer est rĆ©cupĆ©rĆ© au fur et Ć  mesure, cette premiĆØre Ć©tape ayant une durĆ©e comprise entre 5 minutes et plusieurs heures.According to the present invention, this method comprises a first step at a first pressure of less than 7 bar during which the product to be dehydrated is heated to a temperature below the evaporation temperature of the liquid to be removed and the liquid to be removed is recovered. progressively, this first step having a duration of between 5 minutes and several hours.

Il est proposƩ ici de rƩaliser un premier traitement (compression et/ou filtration) Ơ pression peu ƩlevƩe et Ơ basse tempƩrature pendant une longue durƩe. Cette approche originale permet une bonne sƩparation de la phase liquide hors du produit Ơ dƩshydrater tout en minimisant la consommation d'Ʃnergie pour rƩaliser la dƩshydratation correspondante. Le liquide Ʃtant ƩliminƩ au fur et Ơ mesure, il n'est pas chauffƩ inutilement, ce qui permet de limiter la consommation ƩnergƩtique au cours de la mise en oeuvre du procƩdƩ.It is proposed here to perform a first treatment (compression and / or filtration) at low pressure and low temperature for a long time. This original approach allows a good separation of the liquid phase from the product to be dehydrated while minimizing the energy consumption to achieve the corresponding dehydration. As the liquid is gradually removed, it is not heated unnecessarily, which limits the energy consumption during the implementation of the process.

Selon une forme de rĆ©alisation prĆ©fĆ©rĆ©e du procĆ©dĆ© selon la prĆ©sente invention, la premiĆØre pression est comprise entre 1,5 et 4 bars, de prĆ©fĆ©rence autour de 3 bars pour la majoritĆ© des produits pour lesquels le procĆ©dĆ© a Ć©tĆ© testĆ©.According to a preferred embodiment of the process according to the present invention, the first pressure is between 1.5 and 4 bar, preferably around 3 bar for the majority of products for which the process has been tested.

Une forme de rĆ©alisation de la prĆ©sente invention prĆ©voit que le dispositif de filtration et/ou compression comporte une enceinte prĆ©sentant une paroi dont une partie au moins est chauffĆ©e, et que le produit Ć  dĆ©shydrater est chauffĆ© par conduction Ć  partir de la partie chauffĆ©e de la paroi. La partie de la paroi de l'enceinte qui est chauffĆ©e peut ĆŖtre fixe ou mobile. Si la pression est rĆ©alisĆ©e par un piston, des plateaux ou par d'autres Ć©lĆ©ments, on peut prĆ©voir que les moyens permettant d'exercer une pression sur le produit Ć  dĆ©shydrater sont chauffĆ©s. Le chauffage peut ĆŖtre rĆ©alisĆ© par tous moyens : rĆ©sistance Ć©lectrique, fluide caloporteur, rayonnement etc..An embodiment of the present invention provides that the filtration and / or compression device comprises an enclosure having a wall of which at least a portion is heated, and that the product to be dehydrated is heated by conduction from the heated portion of the wall. The portion of the wall of the enclosure that is heated may be fixed or movable. If the pressure is achieved by a piston, trays or other elements, it can be provided that the means for exerting pressure on the product to be dehydrated are heated. Heating can be achieved by any means: electrical resistance, heat transfer fluid, radiation etc.

Pour augmenter la quantitĆ© de liquide sĆ©parĆ© du produit Ć  dĆ©shydrater, le procĆ©dĆ© selon l'invention prĆ©voit que la premiĆØre Ć©tape Ć  basse pression est suivie d'une seconde Ć©tape Ć  une seconde pression, cette seconde pression Ć©tant supĆ©rieure Ć  la premiĆØre pression et infĆ©rieure Ć  30 bars. On rĆ©alise ainsi une sĆ©paration supplĆ©mentaire qui permet d'augmenter le rendement du procĆ©dĆ©. Avec certains produits, comme la bentonite par exemple, cette augmentation de rendement est sensible mais il a Ć©tĆ© remarquĆ© avec certains autres produits que cette seconde Ć©tape Ć  pression plus Ć©levĆ©e ne permettait d'extraire que relativement peu de liquide. Dans cette seconde Ć©tape, la tempĆ©rature reste de prĆ©fĆ©rence infĆ©rieure Ć  la tempĆ©rature de vaporisation du liquide Ć  extraire. Une variante prĆ©fĆ©rĆ©e prĆ©voit que dans la seconde Ć©tape la partie chauffĆ©e de la paroi reste Ć  tempĆ©rature sensiblement constante, cette tempĆ©rature correspondant Ć  la tempĆ©rature de ladite partie chauffĆ©e de la paroi dans le dispositif de filtration et/ou de compression Ć  la fin de la premiĆØre Ć©tape.In order to increase the quantity of liquid separated from the product to be dehydrated, the method according to the invention provides that the first low pressure step is followed by a second step at a second pressure, this second pressure being greater than the first pressure and less than 30 bars. An additional separation is thus achieved which makes it possible to increase the efficiency of the process. With some products, such as bentonite for example, this increase in yield is noticeable but it has been noticed with some other products that this second step at higher pressure could extract relatively little liquid. In this second step, the temperature preferably remains lower than the vaporization temperature of the liquid to be extracted. A preferred variant provides that in the second step the heated portion of the wall remains at a substantially constant temperature, this temperature corresponding to the temperature of said heated portion of the wall in the filtration and / or compression device at the end of the first step.

Dans un procĆ©dĆ© selon l'invention dans lequel le dispositif Ć  dĆ©shydrater est disposĆ© dans une enceinte dont une partie de la paroi est chauffĆ©e, alors, dans la seconde Ć©tape dudit procĆ©dĆ©, la partie chauffĆ©e de la paroi reste de prĆ©fĆ©rence Ć  tempĆ©rature sensiblement constante, cette tempĆ©rature correspondant Ć  la tempĆ©rature de ladite partie chauffĆ©e de la paroi dans le dispositif de filtration et/ou de compression Ć  la fin de la premiĆØre Ć©tape de compression. Lorsque le liquide Ć  Ć©liminer contient majoritairement de l'eau, la partie chauffĆ©e de la paroi est portĆ©e Ć  une tempĆ©rature comprise par exemple entre 40Ā°C et 90Ā°C dans la premiĆØre Ć©tape.In a process according to the invention in which the device to be dehydrated is disposed in an enclosure, part of the wall of which is heated, then, in the second stage of said process, the heated portion of the wall preferably remains at a substantially constant temperature, this temperature corresponding to the temperature of said heated portion of the wall in the filtering device and / or compression at the end of the first compression step. When the liquid to be removed contains mainly water, the heated portion of the wall is brought to a temperature of, for example, between 40 Ā° C. and 90 Ā° C. in the first step.

Le procĆ©dĆ© selon l'invention peut Ć©galement comporter, avant la premiĆØre Ć©tape, une Ć©tape de dĆ©shydratation Ć  tempĆ©rature ambiante, sans apport de chaleur, Ć  une pression correspondant Ć  la premiĆØre pression.The method according to the invention may also comprise, before the first step, a dehydration step at room temperature, without the addition of heat, at a pressure corresponding to the first pressure.

Le procĆ©dĆ© selon l'invention permet d'obtenir des rendements supĆ©rieurs avec une consommation Ć©nergĆ©tique moindre lorsqu'il est appliquĆ© par exemple au prĆ©traitement d'une biomasse humide, Ć  l'exclusion du bois. La biomasse humide traitĆ©e ici peut ĆŖtre par exemple des cĆ©rĆ©ales, des plantes fourragĆØres, des plantes lĆ©gumineuses, des plantes Ć  fibres, des plantes olĆ©agineuses, des plantes Ć  colorant, .... Parmi ces plantes, on peut ainsi par exemple citer Ć  titre d'exemples non limitatifs la luzerne, le ray-grass, le soja et le pastel. Lorsque le procĆ©dĆ© selon l'invention est appliquĆ© Ć  un prĆ©traitement de biomasse humide, cette biomasse humide, aprĆØs dĆ©shydratation mĆ©canique assistĆ©e thermiquement, peut par exemple subir une Ć©tape finale de sĆ©chage thermique dans un sĆ©cheur, le sĆ©cheur Ć©tant alors avantageusement muni d'un Ć©changeur de chaleur en sortie, et l'Ć©nergie des buĆ©es rĆ©cupĆ©rĆ©e dans l'Ć©changeur de chaleur Ć©tant au moins partiellement utilisĆ©e pour rĆ©aliser un chauffage lors des Ć©tapes prĆ©cĆ©dentes du procĆ©dĆ©. De cette maniĆØre, il est possible d'optimiser le bilan Ć©nergĆ©tique de toute la chaĆ®ne de traitement de la biomasse mise en oeuvre dans le procĆ©dĆ©.The process according to the invention makes it possible to obtain higher yields with a lower energy consumption when it is applied, for example, to the pretreatment of a wet biomass, excluding wood. The wet biomass treated here can be, for example, cereals, forage plants, leguminous plants, fiber plants, oleaginous plants, dye plants, etc. Among these plants, it is for example possible to mention non-limiting examples include alfalfa, ryegrass, soybean and pastel. When the process according to the invention is applied to a pretreatment of wet biomass, this wet biomass, after thermally assisted mechanical dehydration, may for example undergo a final step of thermal drying in a dryer, the dryer then being advantageously equipped with a heat exchanger heat output, and the fog energy recovered in the heat exchanger being at least partially used to achieve heating in the previous steps of the method. In this way, it is possible to optimize the energy balance of the entire treatment chain of the biomass used in the process.

Un procĆ©dĆ© selon l'invention peut aussi ĆŖtre appliquĆ© par exemple Ć  la dĆ©shydratation de dĆ©chets liquides ou pĆ¢teux, Ć  l'exclusion des boues rĆ©siduaires urbaines et des boues d'eau potable. Il peut s'agir ici de boues industrielles telles par exemple des boues de papeterie ou bien encore d'un dĆ©chet tel de la bentonite sodique usagĆ©e.A method according to the invention can also be applied for example to the dehydration of liquid or pasty waste, excluding urban waste sludge and drinking water sludge. This may be industrial sludge such as for example paper sludge or even a waste such as sodium bentonite used.

Un procĆ©dĆ© selon l'invention est Ć©galement bien adaptĆ© Ć  l'extraction de jus vert Ć  partir d'une biomasse humide, Ć  l'exclusion du bois. Il s'agit ici par exemple d'extraire un jus riche en protĆ©ines d'une plante telle la luzerne. Le liquide Ć©vacuĆ© au cours de la dĆ©shydratation est alors valorisĆ© et n'est pas un dĆ©chet. Pour favoriser dans ce procĆ©dĆ© la qualitĆ© du jus vert issu de la dĆ©shydratation mĆ©canique assistĆ©e thermiquement, la tempĆ©rature de la paroi chauffĆ©e reste avantageusement infĆ©rieure Ć  60Ā°C. De prĆ©fĆ©rence, la tempĆ©rature des parois chauffĆ©es est de l'ordre de 50Ā°C (+/- 2Ā°C).A method according to the invention is also well suited to the extraction of green juice from a wet biomass, excluding wood. This is for example to extract a high protein juice from a plant such as alfalfa. The liquid discharged during the dehydration is then recovered and is not a waste. To promote in this process the quality of green juice from thermally assisted mechanical dehydration, the temperature of the heated wall advantageously remains below 60 Ā° C. Preferably, the temperature of the heated walls is of the order of 50 Ā° C (+/- 2 Ā° C).

Des dƩtails et avantages de la prƩsente invention ressortiront mieux de la description qui suit, faite en rƩfƩrence aux dessins schƩmatiques annexƩs sur lesquels :

  • La figure 1 reprĆ©sente, en perspective avec une coupe partielle, une cellule de filtration/compression utilisĆ©e pour la mise en oeuvre d'un procĆ©dĆ© selon l'invention,
  • La figure 2 illustre l'influence de la tempĆ©rature lorsque le procĆ©dĆ© selon l'invention est utilisĆ© avec de la bentonite,
  • La figure 3 montre l'influence de la pression dans le procĆ©dĆ© selon l'invention avec de la bentonite,
  • La figure 4 montre l'influence de la tempĆ©rature avec le procĆ©dĆ© selon l'invention pour de la luzerne,
  • La figure 5 montre l'influence de la tempĆ©rature dans un procĆ©dĆ© selon l'invention appliquĆ© Ć  une boue de papeterie,
  • La figure 6 montre l'influence de la pression dans le procĆ©dĆ© selon l'invention appliquĆ© Ć  une boue de papeterie,
  • La figure 7 illustre la cinĆ©tique de production de jus vert lors d'une dĆ©shydratation mĆ©canique selon la prĆ©sente invention, et
  • La figure 8 illustre schĆ©matiquement un procĆ©dĆ© de dĆ©shydratation mettant en oeuvre une dĆ©shydratation mĆ©canique et un sĆ©chage thermique.
Details and advantages of the present invention will emerge more clearly from the description which follows, made with reference to the appended diagrammatic drawings in which:
  • The figure 1 represents, in perspective with a partial section, a filtration / compression cell used for carrying out a process according to the invention,
  • The figure 2 illustrates the influence of temperature when the process according to the invention is used with bentonite,
  • The figure 3 shows the influence of the pressure in the process according to the invention with bentonite,
  • The figure 4 shows the influence of temperature with the process according to the invention for alfalfa,
  • The figure 5 shows the influence of temperature in a process according to the invention applied to a stationary sludge,
  • The figure 6 shows the influence of the pressure in the process according to the invention applied to a stationary sludge,
  • The figure 7 illustrates the kinetics of green juice production during mechanical dewatering according to the present invention, and
  • The figure 8 schematically illustrates a dehydration process employing mechanical dehydration and thermal drying.

La figure 1 reprĆ©sente une cellule de filtration/compression pouvant ĆŖtre utilisĆ©e pour la mise en oeuvre d'un procĆ©dĆ© selon l'invention. Cette cellule comporte d'une part un cylindre 2 destinĆ© Ć  recevoir un produit Ć  dĆ©shydrater et d'autre part un piston 4 adaptĆ© au cylindre 2 de maniĆØre Ć  pouvoir coulisser dans celui-ci. Le cylindre 2 est par exemple usinĆ© dans du polytĆ©trafluoroĆ©thylĆØne, connu sous la marque tĆ©flon et qui est un matĆ©riau isolant thermique. Le piston 4 quant Ć  lui peut ĆŖtre par exemple rĆ©alisĆ© en cuivre. Des rĆ©sistances Ć©lectriques 6 sont intĆ©grĆ©es dans le piston 4 de maniĆØre Ć  pouvoir chauffer celui-ci.The figure 1 represents a filtration / compression cell that can be used for carrying out a method according to the invention. This cell comprises firstly a cylinder 2 for receiving a product to be dewatered and secondly a piston 4 adapted to the cylinder 2 so as to slide therein. The cylinder 2 is for example machined in polytetrafluoroethylene, known under the brand Teflon and which is a thermal insulating material. The piston 4 can be made of copper, for example. Electrical resistors 6 are integrated in the piston 4 so as to heat it.

Une enveloppe extƩrieure 8, par exemple rƩalisƩe en acier, assure la rƩsistance mƩcanique de l'ensemble.An outer casing 8, for example made of steel, provides the mechanical strength of the assembly.

Au fond du cylindre 2 se trouve un mƩdia filtrant 10 qui comporte d'une part un filtre en microfibres de verre dƩposƩ sur une grille rƩalisƩe par exemple dans un matƩriau de marque tƩflon. On remarque sous le mƩdia filtrant la prƩsence d'un collecteur 12 de liquide. Une sortie 14 est prƩvue pour l'Ʃvacuation du liquide collectƩ au niveau du collecteur 12.At the bottom of the cylinder 2 is a filter medium 10 which comprises firstly a glass microfiber filter deposited on a grid made for example of a teflon brand material. It is noted under the filter media the presence of a collector 12 of liquid. An outlet 14 is provided for the evacuation of the liquid collected at the collector 12.

Une cellule de filtration/compression telle celle reprĆ©sentĆ©e sur la figure 1 est destinĆ©e Ć  ĆŖtre insĆ©rĆ©e dans une presse hydraulique (non reprĆ©sentĆ©e), par exemple une presse hydraulique de marque Carver.A filtration / compression cell such as that shown on the figure 1 is intended to be inserted in a hydraulic press (not shown), for example a Carver hydraulic press.

Pour la mise en oeuvre du procƩdƩ, le produit Ơ dƩshydrater est versƩ dans le cylindre 2 de la cellule de filtration/compression. Le piston 4 est ensuite introduit dans le cylindre 2 et vient comprimer le produit Ơ dƩshydrater. Une pression constante est alors exercƩe par ce piston 4 sur le produit Ơ dƩshydrater se trouvant dans le cylindre 2. Un filtrat s'Ʃcoule Ơ travers le mƩdia filtrant 10 vers le collecteur 12 et est ƩvacuƩ par la sortie 14.For the implementation of the process, the product to be dehydrated is poured into the cylinder 2 of the filtration / compression cell. The piston 4 is then introduced into the cylinder 2 and compresses the product to be dehydrated. A constant pressure is then exerted by this piston 4 on the product to be dehydrated in the cylinder 2. A filtrate flows through the filter medium 10 to the collector 12 and is discharged through the outlet 14.

Le procƩdƩ de dƩshydratation mƩcanique assistƩ thermiquement selon l'invention comporte deux phases principales :

  • une premiĆØre phase de dĆ©shydratation Ć  une premiĆØre pression P1 au cours de laquelle le piston est chauffĆ© pour ĆŖtre Ć  une tempĆ©rature T, et
  • une seconde phase de dĆ©shydratation Ć  pression plus Ć©levĆ©e P2 > P1. La tempĆ©rature du piston T reste ici identique Ć  sa tempĆ©rature Ć  la fin de la premiĆØre phase.
The thermally assisted mechanical dehydration process according to the invention comprises two main phases:
  • a first phase of dehydration at a first pressure P1 during which the piston is heated to be at a temperature T, and
  • a second phase of dehydration at higher pressure P2> P1. The temperature of the piston T remains here identical to its temperature at the end of the first phase.

La premiĆØre phase peut ĆŖtre subdivisĆ©e en deux sous-phases : tout d'abord une premiĆØre sous-phase oĆ¹ le produit Ć  dĆ©shydrater est mis sous pression Ć  tempĆ©rature ambiante et une seconde sous-phase oĆ¹ le piston monte en tempĆ©rature jusqu'Ć  atteindre la tempĆ©rature T.The first phase can be subdivided into two sub-phases: all firstly a first sub-phase where the product to be dehydrated is pressurized at ambient temperature and a second sub-phase where the piston rises in temperature until reaching the temperature T.

Le procƩdƩ selon l'invention a ƩtƩ appliquƩ Ơ titre d'exemples non limitatifs Ơ de la bentonite, Ơ de la luzerne et Ơ des boues de papeterie. Pour la bentonite et la luzerne, la pression P1 a ƩtƩ choisie Ơ 3 bars tandis que, pour les boues de papeterie, la pression P1 vaut 1,78 bar. Ces valeurs correspondent Ơ un mode de rƩalisation prƩfƩrƩ et sont donnƩes ici Ơ titre illustratif et non limitatif.The process according to the invention has been applied as non-limiting examples to bentonite, alfalfa and paper mills. For bentonite and alfalfa, the pressure P1 was chosen at 3 bar while, for the paper sludge, the pressure P1 is 1.78 bar. These values correspond to a preferred embodiment and are given here by way of illustration and not limitation.

La pression P2 au cours de la deuxiĆØme phase est choisie supĆ©rieure Ć  la pression P1 en restant toutefois infĆ©rieure Ć  30 bars.The pressure P2 during the second phase is chosen to be greater than the pressure P1 while remaining less than 30 bars.

Les figures 2 et 3 montrent les rĆ©sultats obtenus avec de la bentonite. Ce matĆ©riau minĆ©ral est utilisĆ© dans le domaine du gĆ©nie civil pour fixer des sols et des talus lors de travaux. Il s'agit d'une argile qui a subi un traitement pour lui confĆ©rer des propriĆ©tĆ©s plastiques particuliĆØres. En fin de chantier, la bentonite est rĆ©cupĆ©rĆ©e et rĆ©utilisĆ©e tant que ses propriĆ©tĆ©s rhĆ©ologiques ne sont pas altĆ©rĆ©es. En fin de cycle, le produit est stockĆ©. On remarque que la bentonite ainsi stockĆ©e contient environ 90% d'eau. Il est donc intĆ©ressant de dĆ©shydrater cette bentonite d'une part pour limiter sa masse durant son transport et d'autre part pour limiter son volume.The Figures 2 and 3 show the results obtained with bentonite. This mineral material is used in the field of civil engineering to fix soil and embankments during construction. It is a clay that has been treated to give it special plastic properties. At the end of the worksite, the bentonite is recovered and reused as long as its rheological properties are not altered. At the end of the cycle, the product is stored. It is noted that the bentonite thus stored contains about 90% water. It is therefore interesting to dehydrate this bentonite on the one hand to limit its mass during transport and on the other hand to limit its volume.

La figure 2 illustre le pourcentage massique d'eau Ć©liminĆ©e pendant la premiĆØre phase, en fonction de la tempĆ©rature du piston 4. La durĆ©e de cette premiĆØre phase est fixĆ©e ici Ć  3 heures. De mĆŖme que les autres valeurs numĆ©riques indiquĆ©es, cette valeur est donnĆ©e Ć  titre illustratif et non limitatif. Avec une telle durĆ©e, un gradient de tempĆ©rature s'Ć©tablit dans le produit Ć  dĆ©shydrater se trouvant dans la cellule de filtration/compression. Le chauffage du produit Ć  dĆ©shydrater est rĆ©alisĆ© ici par conduction. En disposant des rĆ©sistances chauffantes dans les parois du cylindre 2, on pourrait obtenir une montĆ©e en tempĆ©rature du produit Ć  dĆ©shydrater plus rapide et ainsi diminuer la durĆ©e de la phase 1. D'autres modes de chauffage peuvent ĆŖtre envisagĆ©s. On peut ainsi notamment prĆ©voir de chauffer le produit avant de l'introduire dans la cellule de filtration/compression. Cette solution n'est pas prĆ©fĆ©rĆ©e car elle oblige Ć  chauffer de l'eau (ou autre liquide) qui est ensuite Ć©liminĆ©e - chaude - lors de la mise sous pression du produit Ć  dĆ©shydrater dans la cellule de filtration/compression.The figure 2 illustrates the mass percentage of water removed during the first phase, as a function of the temperature of the piston 4. The duration of this first phase is set here to 3 hours. As well as the other numerical values indicated, this value is given for illustrative and not limiting. With such a duration, a temperature gradient is established in the product to be dehydrated in the filtration / compression cell. The heating of the product to be dehydrated is carried out here by conduction. By having heating resistors in the walls of the cylinder 2, it could be possible to increase the temperature of the product to be dehydrated faster and thus reduce the duration of the phase 1. Other heating modes can be envisaged. In particular, it is possible to heat the product before introducing it into the filtration / compression cell. This solution is not preferred because it requires heating water (or other liquid) which is then removed - hot - during the pressurization of the product to be dehydrated in the filtration / compression cell.

Le pourcentage massique d'eau Ć©liminĆ©e est calculĆ© de la maniĆØre suivante : il s'agit du rapport entre la masse d'eau sĆ©parĆ©e durant une phase du procĆ©dĆ© et la masse totale d'eau dans le matĆ©riau. Ce rapport est toujours infĆ©rieur Ć  1 et est exprimĆ© en pourcentage sur les figures.The mass percentage of water removed is calculated in the same way next: it is the ratio between the mass of water separated during a phase of the process and the total mass of water in the material. This ratio is always less than 1 and is expressed as a percentage in the figures.

La figure 2 reprĆ©sente le pourcentage massique d'eau Ć©liminĆ©e au bout de 3 heures pour diffĆ©rentes tempĆ©ratures du piston 4. La tempĆ©rature T du piston varie ici entre 21 Ā°C et 90Ā°C. On constate que la quantitĆ© d'eau Ć©liminĆ©e croĆ®t avec la tempĆ©rature du piston. Pour des tempĆ©ratures de l'ordre de 80 Ć  90Ā°C, on remarque que 70% de l'eau contenue dans la bentonite est Ć©liminĆ©e. Selon les besoins de l'utilisateur, cette rĆ©duction de masse de la bentonite peut ĆŖtre suffisante.The figure 2 represents the mass percentage of water removed after 3 hours for different temperatures of the piston 4. The temperature T of the piston varies here between 21 Ā° C and 90 Ā° C. It is found that the amount of water removed increases with the temperature of the piston. For temperatures of the order of 80 to 90 Ā° C, it is noted that 70% of the water contained in the bentonite is removed. Depending on the needs of the user, this mass reduction of the bentonite may be sufficient.

Dans le cas de figure reprĆ©sentĆ© sur la figure 3, on a choisi de fixer la tempĆ©rature du piston Ć  80Ā°C. Comme il ressort de la figure 2, 70% de l'eau est Ć©liminĆ©e au cours de la premiĆØre phase. Cette valeur est reprise sur la figure 3. Cette figure montre quelle quantitĆ© d'eau peut ĆŖtre encore Ć©liminĆ©e durant la seconde phase en fonction de la pression appliquĆ©e au produit Ć  dĆ©shydrater durant cette seconde phase. La durĆ©e de cette seconde phase est ici de 2 heures.In the case of figure represented on the figure 3 it was chosen to set the temperature of the piston at 80 Ā° C. As is apparent from the figure 2 70% of the water is removed during the first phase. This value is taken from the figure 3 . This figure shows how much water can be removed during the second phase depending on the pressure applied to the product to be dehydrated during this second phase. The duration of this second phase is here of 2 hours.

Sur la gauche de la figure 3, on a choisi P2 = 7 bars tandis que la partie droite de cette figure, on a choisi P2 = 26 bars. On remarque ici que la seconde phase permet de retirer une quantitƩ d'eau assez importante (environ 25% de l'eau contenue initialement dans le produit). On remarque Ʃgalement qu'Ơ 26 bars presque toute l'eau contenue dans la bentonite est ƩliminƩe. Il est donc a priori inutile d'essayer d'augmenter la pression P2.On the left of the figure 3 , we chose P2 = 7 bars while the right part of this figure, we chose P2 = 26 bars. It should be noted here that the second phase makes it possible to withdraw a fairly large quantity of water (approximately 25% of the water initially contained in the product). It is also noted that at 26 bar almost all the water contained in the bentonite is removed. It is therefore a priori useless to try to increase the pressure P2.

La prĆ©sente invention peut Ć©galement ĆŖtre mise en oeuvre avec de la luzerne. Parmi les pratiques impliquant une conservation du fourrage de luzerne, la dĆ©shydratation industrielle est une alternative Ć  l'ensilage et Ć  la dĆ©shydratation au champ. La dĆ©shydratation permet de prĆ©server au mieux les qualitĆ©s initiales du fourrage. Ce procĆ©dĆ© de transformation s'est fortement dĆ©veloppĆ© en France qui est devenu l'un des principaux producteurs de fourrage dĆ©shydratĆ© en Europe. La production de luzerne dĆ©shydratĆ©e est actuellement de l'ordre de 12 Ć  15 tonnes de matiĆØre sĆØche par hectare et par an. Toutefois, le coĆ»t actuel de l'Ć©nergie pĆ©nalise fortement ce mode de traitement.The present invention can also be implemented with alfalfa. Among the practices involving alfalfa forage conservation, industrial dewatering is an alternative to silage and dehydration in the field. Dehydration allows the best preservation of the initial qualities of the forage. This process of transformation has developed strongly in France, which has become one of the leading producers of dehydrated fodder in Europe. Dehydrated alfalfa production is currently in the range of 12 to 15 tonnes of dry matter per hectare per year. However, the current cost of energy strongly penalizes this mode of treatment.

La dĆ©shydratation de la luzerne est actuellement rĆ©alisĆ©e par des procĆ©dĆ©s dits "en voie sĆØche", c'est-Ć -dire en mettant en oeuvre exclusivement un sĆ©chage thermique et conduisant Ć  la valorisation du tourteau en alimentation animale, ou bien des procĆ©dĆ©s, dits "en voie humide". Ces derniers mettent en oeuvre une Ć©tape prĆ©alable de dĆ©shydratation par presse Ć  vis. Ces procĆ©dĆ©s "en voie humide" permettent de sĆ©parer une phase aqueuse (jus vert), qui est riche en protĆ©ines et en pigments naturels. De tels procĆ©dĆ©s permettent donc d'obtenir d'une part le tourteau pour l'alimentation animale et d'autre part de valoriser le jus vert en alimentation animale ou humaine.The dehydration of alfalfa is currently carried out by so-called "dry processes", that is to say by implementing exclusively thermal drying and leading to the development of the meal in animal feed, or processes, called "wet". The latter implement a preliminary step of dehydration by screw press. These "wet" processes make it possible to separate an aqueous phase (green juice), which is rich in proteins and natural pigments. Such processes thus make it possible to obtain, on the one hand, the meal for animal feed and, on the other hand, to enhance the use of green juice in animal or human nutrition.

Le procƩdƩ selon l'invention permet d'augmenter le rendement de la sƩparation.The process according to the invention makes it possible to increase the yield of the separation.

Pour l'application du procĆ©dĆ© Ć  de la luzerne, la durĆ©e de la premiĆØre phase a Ć©tĆ© fixĆ©e Ć  4 heures. Celle de la seconde phase a Ć©tĆ© fixĆ©e quant Ć  elle Ć  2 heures.For the application of the process to alfalfa, the duration of the first phase was fixed at 4 hours. That of the second phase was fixed at 2 hours.

Sur les dessins, seuls les rĆ©sultats de la sĆ©paration Ć  l'issue de la phase 1 sont reprĆ©sentĆ©s. Il a Ć©tĆ© remarquĆ© que la phase aqueuse (le jus vert) est principalement Ć©liminĆ©e pendant la premiĆØre phase du procĆ©dĆ© et que seules de faibles quantitĆ©s d'eau (jus vert) sont Ć©liminĆ©es au cours de la seconde phase du procĆ©dĆ©. Pour la luzerne, l'impact de la tempĆ©rature est prĆ©pondĆ©rant comme le montre notamment la figure 4. On remarque ainsi que pour une tempĆ©rature de 80Ā°C, il est possible d'extraire 80% de l'eau contenue dans la luzerne.In the drawings, only the results of the separation at the end of phase 1 are shown. It has been noticed that the aqueous phase (the green juice) is mainly removed during the first phase of the process and that only small amounts of water (green juice) are removed during the second phase of the process. For alfalfa, the impact of temperature is preponderant, as shown in particular by figure 4 . We note that for a temperature of 80 Ā° C, it is possible to extract 80% of the water contained in alfalfa.

La siccitĆ© est un paramĆØtre utilisĆ© pour indiquer le pourcentage massique de matiĆØre sĆØche contenue dans un produit. La siccitĆ© d'un produit est donc le rapport entre la masse sĆØche contenue dans ce produit et la masse totale du produit. Ici Ć©galement, il s'agit d'un rapport infĆ©rieur Ć  1 qui est exprimĆ© en pourcentage. La siccitĆ© peut ĆŖtre Ć©galement considĆ©rĆ©e comme le rapport de la masse sĆØche du produit sur la somme de la masse sĆØche et de la masse d'eau de ce produit.Dryness is a parameter used to indicate the percentage by mass of dry matter contained in a product. The dryness of a product is therefore the ratio between the dry mass contained in this product and the total mass of the product. Here too, it is a ratio of less than 1 which is expressed as a percentage. Dryness can also be considered as the ratio of the dry mass of the product to the sum of the dry mass and the water content of this product.

Il est intƩressant ici de comparer le procƩdƩ selon l'invention avec un procƩdƩ classiquement utilisƩ pour dƩshydrater de la luzerne "en voie humide".It is interesting here to compare the process according to the invention with a method conventionally used to dehydrate alfalfa "wet".

On suppose que la luzerne prĆ©sente une siccitĆ© initiale de 20%. Des procĆ©dĆ©s classiques de pressage permettent d'obtenir une siccitĆ© de 32,5%. AprĆØs sĆ©chage dans un sĆ©cheur thermique, la siccitĆ© finale est d'environ 87%.Alfalfa is assumed to have an initial dryness of 20%. Conventional pressing methods make it possible to obtain a dryness of 32.5%. After drying in a thermal dryer, the final dryness is about 87%.

Avec le procƩdƩ de dƩshydratation selon l'invention, il est possible d'augmenter la siccitƩ intermƩdiaire de la luzerne, avant son introduction dans un sƩcheur thermique. Les rƩsultats obtenus en laboratoire montrent que l'on peut obtenir une siccitƩ intermƩdiaire de 62,5% en utilisant un procƩdƩ de dƩshydratation mƩcanique assistƩe thermiquement selon l'invention. Ceci permet d'une part de sƩparer une quantitƩ de liquide (jus vert) bien plus importante et d'autre part de limiter l'Ʃnergie nƩcessaire pour atteindre l'objectif de 87% de siccitƩ dans un sƩcheur thermique.With the dehydration process according to the invention, it is possible to increase the intermediate dryness of alfalfa, before its introduction into a thermal dryer. The results obtained in the laboratory show that an intermediate dryness of 62.5% can be obtained by using a thermally assisted mechanical dehydration process according to the invention. This makes it possible, on the one hand, to separate a much larger amount of liquid (green juice) and, on the other hand, to limit the energy required to reach the 87% dryness objective in a thermal dryer.

En effet, si l'on raisonne sur la base d'une tonne de luzerne dĆ©shydratĆ©e Ć  l'heure, avec les donnĆ©es indiquĆ©es plus haut, selon un procĆ©dĆ© de l'art antĆ©rieur, la quantitĆ© de liquide (jus vert) sĆ©parĆ© par voie mĆ©canique (pour arriver Ć  la siccitĆ© intermĆ©diaire de 32,5%) s'Ć©lĆØve Ć  380 kg/h et la quantitĆ© d'eau Ć©vaporĆ©e dans le sĆ©cheur thermique pour arriver Ć  une siccitĆ© finale de 87% est de 390 kg/h.Indeed, if one reasons on the basis of a tonne of alfalfa dehydrated per hour, with the data indicated above, according to a process of the prior art, the amount of liquid (green juice) separated by a route mechanical (to achieve the intermediate dryness of 32.5%) is 380 kg / h and the amount of water evaporated in the heat dryer to achieve a final dryness of 87% is 390 kg / h.

En utilisant le procƩdƩ selon l'invention, en partant d'une siccitƩ initiale de 20% pour arriver Ơ une siccitƩ finale de 87%, en passant par une siccitƩ intermƩdiaire de 62,5%, la quantitƩ de liquide (jus vert) produit est de 680 kg/h et la quantitƩ d'eau ƩvaporƩe dans le sƩcheur thermique est de 90 kg/h.Using the process according to the invention, starting from an initial dryness of 20% to reach a final dryness of 87%, passing through an intermediate dryness of 62.5%, the amount of liquid (green juice) produced is 680 kg / h and the amount of water evaporated in the thermal dryer is 90 kg / h.

Cet exemple numĆ©rique (rĆ©aliste) illustre les gains qui peuvent ĆŖtre obtenus pour la dĆ©shydratation de la luzerne. Le gain massique en jus vert est de plus de 75% tandis que la quantitĆ© d'eau Ć  Ć©vaporer est environ divisĆ©e par quatre.This (realistic) numerical example illustrates the gains that can be made for the dehydration of alfalfa. The mass gain in green juice is more than 75% while the amount of water to be evaporated is approximately divided by four.

La figure 7 montre l'influence de la tempƩrature de chauffage sur la cinƩtique d'extraction de jus vert de luzerne. Le procƩdƩ mis en oeuvre pour l'obtention des deux courbes de la figure 7 comporte les Ʃtapes suivantes :

  • dĆ©shydratation Ć  faible pression et Ć  tempĆ©rature ambiante,
  • dĆ©shydratation Ć  faible pression et chauffage du piston, et
  • incrĆ©ment de la pression et maintien de la tempĆ©rature du piston constante (par rapport Ć  l'Ć©tape prĆ©cĆ©dente).
The figure 7 shows the influence of the heating temperature on the extraction kinetics of alfalfa green juice. The process used to obtain the two curves of the figure 7 includes the following steps:
  • dehydration at low pressure and at room temperature,
  • low pressure dehydration and piston heating, and
  • Increasing the pressure and maintaining the constant piston temperature (compared to the previous step).

Des expĆ©riences ont montrĆ© que pour obtenir un jus vert riche en protĆ©ines ainsi qu'un bon rendement, la tempĆ©rature de la paroi chauffĆ©e Ć©tait de prĆ©fĆ©rence de l'ordre de 50Ā°C.Experiments have shown that to obtain a protein-rich green juice and a good yield, the temperature of the heated wall is preferably of the order of 50 Ā° C.

La figure 8 illustre une filiĆØre de dĆ©shydratation du tourteau de luzerne. Deux Ć©tapes sont reprĆ©sentĆ©es ici : une premiĆØre Ć©tape de dĆ©shydratation mĆ©canique et une Ć©tape de sĆ©chage thermique. Avant la premiĆØre Ć©tape, la siccitĆ© de la luzerne est Sinitiale, entre les deux Ć©tapes elle est SintermĆ©diaire et aprĆØs la seconde Ć©tape, elle est Sfinale.The figure 8 illustrates a dehydration pathway for alfalfa cake. Two stages are represented here: a first stage of mechanical dehydration and a stage of thermal drying. Before the first step, the dryness of the alfalfa is S initial , between the two stages it is S intermediate and after the second stage, she is S final .

On considĆØre que l'Ć©nergie fournie lors de la premiĆØre Ć©tape est X1, exprimĆ©e en kWh par tonne d'eau sĆ©parĆ©e et que l'Ć©nergie fournie lors de la seconde Ć©tape est X2, exprimĆ©e en kWh par tonne d'eau sĆ©parĆ©eIt is considered that the energy supplied in the first step is X 1 , expressed in kWh per ton of separated water and that the energy supplied in the second step is X 2 , expressed in kWh per ton of separate water.

La filiĆØre conventionnelle, selon l'art antĆ©rieur Ć  la prĆ©sente invention, comporte :

  • une sĆ©paration mĆ©canique, pour laquelle il est d'usage de considĆ©rer que la consommation Ć©nergĆ©tique d'un filtre presse est comprise entre 1 et 10 kWh par tonne d'eau sĆ©parĆ©e, c'est-Ć -dire que X1 est compris entre 1 et 10. Une consommation de 10 kWh/t d'eau sĆ©parĆ©e a Ć©tĆ© retenue ici (soit X1 = 10).
  • un sĆ©chage thermique conventionnellement rĆ©alisĆ© dans un sĆ©cheur de type four tournant. Le fluide caloporteur entre dans le four Ć  une tempĆ©rature de 700 Ć  800Ā°C et ressort avec une tempĆ©rature supĆ©rieure Ć  100Ā°C. La consommation Ć©nergĆ©tique de ce type d'installation est estimĆ©e Ć  environ 800 kWh/t d'eau Ć©vaporĆ©e, soit X2 = 800. Il est connu ici d'utiliser par exemple un prĆ©-sĆ©cheur Ć  basse tempĆ©rature, utilisant de l'air neuf Ć  70Ā°C prĆ©chauffĆ© dans un Ć©changeur air/eau grĆ¢ce Ć  la condensation des buĆ©es sortant du four tournant. Un tel prĆ©-sĆ©cheur a Ć©tĆ© dĆ©veloppĆ© pour rĆ©duire la consommation Ć©nergĆ©tique associĆ©e Ć  la sĆ©paration thermique. La consommation globale du prĆ©-sĆ©cheur et du four tournant est alors d'environ 580 kWh/t d'eau Ć©vaporĆ©e (X2 = 580), la tempĆ©rature d'entrĆ©e du fluide caloporteur dans le four tournant devant ĆŖtre abaissĆ©e Ć  400Ā°C.
The conventional die, according to the prior art to the present invention, comprises:
  • a mechanical separation, for which it is customary to consider that the energy consumption of a filter press is between 1 and 10 kWh per tonne of water separated, that is to say that X 1 is between 1 and 10. A consumption of 10 kWh / t of separated water was retained here (ie X 1 = 10).
  • conventional thermal drying in a rotary kiln type dryer. The heat transfer fluid enters the oven at a temperature of 700 to 800 Ā° C and exits with a temperature above 100 Ā° C. The energy consumption of this type of installation is estimated at about 800 kWh / t of evaporated water, ie X 2 = 800. It is known here to use for example a low-temperature pre-dryer, using air Nine at 70 Ā° C preheated in an air / water heat exchanger due to the condensation of steam coming out of the rotating furnace. Such a pre-dryer has been developed to reduce the energy consumption associated with thermal separation. The overall consumption of the pre-dryer and the rotary kiln is then about 580 kWh / t of evaporated water (X 2 = 580), the inlet temperature of the heat transfer fluid in the rotary kiln to be lowered to 400 Ā° C. .

En supposant un dĆ©bit de luzerne d'une tonne par heure, une siccitĆ© Sinitiale de la plante de 20%, une siccitĆ© aprĆØs dĆ©shydratation mĆ©canique SintermĆ©diaire de 32.5% et une siccitĆ© finale Sfinale aprĆØs sĆ©chage thermique de 87%, la puissance consommĆ©e sur la filiĆØre conventionnelle s'Ć©lĆØve Ć  312,25 kW pour la filiĆØre intĆ©grant le four tournant et Ć  227,44 kW pour la filiĆØre intĆ©grant le prĆ©-sĆ©cheur en amont du four tournant. Ces rĆ©sultats sur la filiĆØre globale peuvent Ć©galement s'exprimer en terme de consommation spĆ©cifique, ce qui donne 405,45 kWh/t d'eau pour la filiĆØre intĆ©grant le four tournant et 295,33 kWh/t d'eau pour la filiĆØre intĆ©grant le prĆ©-sĆ©cheur en amont du four tournant.Assuming an alfalfa flow rate of one tonne per hour, an initial S dryness of the plant of 20%, a dryness after mechanical dehydration S intermediate of 32.5% and a final dryness S final after thermal drying of 87%, the power consumed on the conventional sector amounts to 312.25 kW for the sector incorporating the rotary kiln and 227.44 kW for the die integrating the pre-dryer upstream of the rotary kiln. These results on the global sector can also be expressed in terms of specific consumption, which gives 405.45 kWh / t of water for the sector integrating the rotary kiln and 295.33 kWh / t of water for the integrated sector. the pre-dryer upstream of the rotary kiln.

Dans une filiĆØre selon la prĆ©sente invention, le filtre presse est remplacĆ© par un dispositif mettant en oeuvre un procĆ©dĆ© de dĆ©shydratation assistĆ© thermiquement tel que dĆ©crit par exemple plus haut. La consommation d'Ć©nergie associĆ©e Ć  cette sĆ©paration mĆ©canique assistĆ©e thermiquement a Ć©tĆ© dĆ©terminĆ©e grĆ¢ce au pilote de laboratoire dĆ©crit plus haut. Les valeurs sont reportĆ©es dans le tableau suivant pour diffĆ©rents tempĆ©ratures de paroi du piston. Tableau 1 Consommation Ć©nergĆ©tique du procĆ©dĆ© de dĆ©shydratation assistĆ©e TempĆ©rature de paroi (Ā°C) Consommation Ć©nergĆ©tique (kWh/t jus sĆ©parĆ©) 50 121,08 70 150,83 In a die according to the present invention, the filter press is replaced by a device implementing a thermally assisted dehydration process as described for example above. Energy consumption associated with this mechanical assisted mechanical separation was determined by the laboratory pilot described above. The values are shown in the following table for different piston wall temperatures. <b> Table 1 Energy consumption of assisted dehydration process </ b> Wall temperature (Ā° C) Energy consumption (kWh / t separate juice) 50 121.08 70 150.83

Les valeurs dans ce tableau sont probablement un peu surƩvaluƩes.The values in this table are probably a bit overvalued.

Avec une base de calcul identique, Ć  savoir un dĆ©bit de luzerne d'une tonne par heure, une siccitĆ© initiale Sinitiale de la plante de 20% et une siccitĆ© finale Sfinale aprĆØs sĆ©chage thermique de 87%, on obtient les consommations suivantes sur la filiĆØre selon la prĆ©sente invention intĆ©grant uniquement le four tournant : Tableau 2 Consommation Ć©nergĆ©tique de la filiĆØre alternative intĆ©grant une dĆ©shydratation mĆ©canique assistĆ©e thermiquement et un sĆ©chage en four tournant TempĆ©rature de paroi (Ā°C) SiccitĆ© intermĆ©diaire SintermĆ©diaire (%) Puissance consommĆ©e (kW) Consommation spĆ©cifique (kWh/t) Gain relatif par rapport Ć  la filiĆØre conventionnelle 50 50,72 204,86 266 34,39 70 56,86 195,24 253,5 37,47 With an identical calculation base, namely a flow rate of alfalfa of one ton per hour, an initial initial dryness S of the plant of 20% and a final dryness S final after thermal drying of 87%, the following consumptions are obtained on the die according to the present invention integrating only the rotary kiln: <b> Table 2 Alternative energy consumption including thermally assisted mechanical dehydration and kiln drying </ b> Wall temperature (Ā° C) Intermediate dryness intermediate S (%) Power consumption (kW) Specific consumption (kWh / t) Relative gain compared to the conventional sector 50 50.72 204.86 266 34.39 70 56.86 195.24 253.5 37.47

On peut noter ici qu'en rĆ©cupĆ©rant l'Ć©nergie contenue dans les buĆ©es sortant du four tournant, par l'intermĆ©diaire d'un Ć©changeur de chaleur, on peut encore diminuer la consommation d'Ć©nergie de la filiĆØre globale.It can be noted here that by recovering the energy contained in the steam coming out of the rotary furnace, by means of a heat exchanger, it is possible to further reduce the energy consumption of the overall system.

Les mĆŖmes calculs effectuĆ©s pour la filiĆØre selon l'invention en intĆ©grant le prĆ©-sĆ©cheur en amont du four tournant conduisent Ć  : Tableau 3 Consommation Ć©nergĆ©tique de la filiĆØre alternative intĆ©grant une dĆ©shydratation mĆ©canique assistĆ©e thermiquement et un prĆ©-sĆ©chage Ć  basse tempĆ©rature en amont du four tournant TempĆ©rature de paroi (Ā°C) SiccitĆ© intermĆ©diaire (%) Puissance consommĆ©e (kW) Consommation spĆ©cifique (kWh/t) Gain relatif par rapport Ć  la filiĆØre conventionnelle 50 50,72 168,7 219 25,83 70 56,86 168,4 218,7 25,94 The same calculations made for the die according to the invention by integrating the pre-dryer upstream of the rotary furnace lead to: <b> Table 3 Alternative energy consumption including thermally assisted mechanical dehydration and low temperature pre-drying upstream of the rotary kiln </ b> Wall temperature (Ā° C) Intermediate SiccitĆ© (%) Power consumption (kW) Specific consumption (kWh / t) Relative gain compared to the conventional sector 50 50.72 168.7 219 25.83 70 56.86 168.4 218.7 25.94

Dans cette configuration, l'Ć©nergie contenue dans les buĆ©es sortant du four tournant a dĆ©jĆ  Ć©tĆ© valorisĆ©e. Les figures 5 et 6 concernent les rĆ©sultats obtenues avec des boues de papeterie en utilisant le procĆ©dĆ© selon l'invention. Ces figures correspondent aux figures 2 et 3 dĆ©crites en application Ć  de la bentonite. La durĆ©e de la premiĆØre phase est ici de 30 minutes tandis que la seconde phase dure 15 minutes.In this configuration, the energy contained in the steam coming out of the rotary kiln has already been enhanced. The figures 5 and 6 relate to the results obtained with stationary sludge using the process according to the invention. These figures correspond to Figures 2 and 3 described in application to bentonite. The duration of the first phase is 30 minutes while the second phase lasts 15 minutes.

La figure 5 montre que, pour des boues de papeterie, l'influence de la tempĆ©rature est relativement faible pour la premiĆØre phase. En effet, alors qu'Ć  25Ā°C le pourcentage massique d'eau Ć©liminĆ©e est de l'ordre de 66%, il n'est que d'environ 67,5% Ć  80Ā°C.The figure 5 shows that, for stationary sludge, the influence of temperature is relatively low for the first phase. Indeed, while at 25 Ā° C the mass percentage of water removed is of the order of 66%, it is only about 67.5% at 80 Ā° C.

La seconde phase est ici intƩressante car elle permet d'Ʃliminer de l'ordre de 15 Ơ 20% d'eau supplƩmentaire. On remarque ici que plus la pression est importante, plus la quantitƩ d'eau sƩparƩe est elle aussi importante. Sur la figure 6, on remarque une variation de quelques pourcents pour le passage d'une pression P2 de 7,3 bars Ơ 10,7 bars.The second phase is interesting here because it allows to eliminate about 15 to 20% additional water. We note here that the higher the pressure, the more the quantity of separated water is also important. On the figure 6 a variation of a few percent is noted for the passage of a pressure P2 of 7.3 bars at 10.7 bars.

Comme il ressort de la description qui prĆ©cĆØde, l'intĆ©rĆŖt du procĆ©dĆ© de dĆ©shydratation mĆ©canique assistĆ©e thermiquement selon l'invention est avĆ©rĆ© pour la dĆ©shydratation de bentonite et de plantes fourragĆØres, telles la luzerne. Des applications dans le domaine agroalimentaire peuvent ĆŖtre envisagĆ©es. Le procĆ©dĆ© dĆ©crit plus haut peut ĆŖtre utilisĆ© pour des plantes, notamment des plantes ligneuses, des lĆ©gumineuses herbacĆ©es, des tomates, des betteraves, etc.. Des sous-produits agricoles ou dĆ©chets verts, peuvent Ć©galement ĆŖtre traitĆ©s avec un procĆ©dĆ© selon l'invention.As is clear from the foregoing description, the interest of the thermally assisted mechanical dehydration process according to the invention is proven for the dehydration of bentonite and forage plants, such as alfalfa. Applications in the agri-food field can be envisaged. The method described above can be used for plants, especially woody plants, herbaceous legumes, tomatoes, beets, etc. Agricultural by-products or green waste, can also be treated with a method according to the invention. .

Dans le domaine minier, d'autres matĆ©riaux que la bentonite peuvent ĆŖtre traitĆ©s. On peut ainsi appliquer le procĆ©dĆ© selon l'invention Ć  de la barytine, de la fluorine ou Ć  divers minĆ©raux argileux.In the mining field, other materials than bentonite can be processed. The process according to the invention can thus be applied to barite, fluorine or various clay minerals.

De maniĆØre gĆ©nĆ©rale, la prĆ©sente invention peut ĆŖtre appliquĆ© Ć  toute biomasse en excluant toutefois de la dĆ©finition qui suit le bois et les boues rĆ©siduaires ainsi que les boues d'eau potable.In general, the present invention can be applied to any biomass but excludes the following definition of wood and sludge as well as drinking water sludge.

Par biomasse on entend :

  • le bois, sous forme de bĆ»ches, granulĆ©s et plaquettes ;
  • les sous-produits du bois qui recouvrent l'ensemble des dĆ©chets produits par l'exploitation forestiĆØre (branchage, Ć©corces, sciures...), par les scieries (sciures, plaquettes...), par les industries de transformation du bois (menuiseries, fabricants de meubles, parquets) et par les fabricants de panneaux ainsi que les emballages tels que les palettes ;
  • les sous-produits de l'industrie tels les boues issues de la pĆ¢te Ć  papier (liqueur noire) et les dĆ©chets des industries agroalimentaires (marcs de raisin et de cafĆ©, pulpes et pĆ©pins de raisin etc.) ;
  • les produits issus de l'agriculture traditionnelle (cĆ©rĆ©ales, olĆ©agineux), rĆ©sidus tels que la paille, la bagasse (rĆ©sidus ligneux de la canne Ć  sucre) et les nouvelles plantations Ć  vocation Ć©nergĆ©tique telles que les taillis Ć  courte rotation (saules, miscanthus, etc.);
  • les dĆ©chets organiques tels que les dĆ©chets urbains comprenant les boues d'Ć©puration, les ordures mĆ©nagĆØres, et les dĆ©chets en provenance de l'agriculture tels que les effluents agricoles. Dans l'art antĆ©rieur, de nombreux Ć©quipements ont Ć©tĆ© dĆ©veloppĆ©s pour intensifier les procĆ©dĆ©s de dĆ©shydratation conventionnels. Toutefois, dans la pratique, les procĆ©dĆ©s dĆ©veloppĆ©s rĆ©pondent globalement Ć  une problĆ©matique diffĆ©rente de celle de la prĆ©sente invention, puisqu'il s'agit fondamentalement de procĆ©dĆ©s de sĆ©chage. La plupart des procĆ©dĆ©s connus reposent sur la technologie du filtre presse. Cette technologie facilite la mise en place d'un dispositif de chauffage. En effet, un filtre presse comporte des plateaux creux permettant la circulation d'un fluide caloporteur. NĆ©anmoins, les plateaux du filtre presse Ć©tant disjoints, la circulation du fluide caloporteur dans chacun des plateaux rend l'installation compliquĆ©e. En outre, les conditions d'utilisation visent Ć  sĆ©cher par contact le gĆ¢teau aprĆØs l'avoir dĆ©shydratĆ© mĆ©caniquement. Des problĆØmes de collage (cuisson) du gĆ¢teau de filtration apparaissent couramment sur les plateaux chauffants et empĆŖchent, ou ralentissent, la vidange du filtre presse. Pour abaisser alors la tempĆ©rature de fonctionnement, un vide partiel doit ĆŖtre rĆ©alisĆ©. L'inconvĆ©nient majeur de cette technologie de l'art antĆ©rieur rĆ©side dans son fonctionnement batch. Une technologie mettant en oeuvre un filtre Ć  bandes a Ć©tĆ© mis au point dans le cadre du sĆ©chage impulsionnel par les papetiers qui maĆ®trisent bien cette technique pour la fabrication du papier. L'apport de chaleur est plus difficile Ć  implĆ©menter car la rotation des rouleaux rend compliquĆ©e la circulation de fluides caloporteurs pour les chauffer. Une alternative consiste cependant Ć  rĆ©aliser un chauffage par induction. Un autre inconvĆ©nient concerne la compacitĆ© du procĆ©dĆ© puisque le produit est disposĆ© en couche mince d'Ć©paisseur infĆ©rieure Ć  1 mm.
Biomass means:
  • wood, in the form of logs, pellets and wafers;
  • wood by-products which cover all the waste produced by logging (branching, bark, sawdust ...), sawmills (sawdust, chips, etc.), by the wood-processing industries ( joineries, furniture manufacturers, flooring) and panel manufacturers as well as packaging such as pallets;
  • industrial by-products such as sludge from paper pulp (black liquor) and waste from agri-food industries (grape and coffee grounds, pulp and grape seed, etc.);
  • products derived from traditional agriculture (cereals, oilseeds), residues such as straw, bagasse (ligneous residues from sugar cane) and new energy plantations such as short-rotation coppices (willow, miscanthus, etc.);
  • organic waste such as urban waste including sewage sludge, household waste, and waste from agriculture such as agricultural effluents. In the prior art, many pieces of equipment have been developed to intensify conventional dewatering processes. However, in practice, the processes developed globally respond to a problem different from that of the present invention, since they are basically drying processes. Most known methods rely on press filter technology. This technology facilitates the installation of a heating device. Indeed, a filter press comprises hollow trays for the circulation of a coolant. Nevertheless, the plates of the filter press being disjoint, the circulation of the coolant in each of the trays makes the installation complicated. In addition, the conditions of use are intended to dry contact the cake after having dehydrated mechanically. Problems of sticking (baking) of the filter cake commonly appear on the heating plates and prevent or slow down the emptying of the filter press. To then lower the operating temperature, a partial vacuum must be realized. The major disadvantage of this technology of the prior art lies in its batch operation. A technology using a band filter has been developed in the context of pulse drying by paper manufacturers who are well versed in this technique for the manufacture of paper. The heat input is more difficult to implement because the rotation of the rollers makes it difficult to circulate heat transfer fluids to heat them. An alternative, however, is to provide induction heating. Another disadvantage relates to the compactness of the process since the product is disposed in a thin layer less than 1 mm thick.

Par opposition, la prĆ©sente invention, dans ce mode de rĆ©alisation prĆ©fĆ©rĆ©, repose sur deux Ć©tapes de sĆ©paration assistĆ©es thermiquement : une premiĆØre Ć©tape, de filtration ou de compression selon le matĆ©riau dĆ©shydratĆ©, Ć  basse pression (de l'ordre de 3 bars dans un mode de rĆ©alisation prĆ©fĆ©rĆ©) suivie d'une Ć©tape de sĆ©paration Ć  plus haute pression, la tempĆ©rature du piston restant constante.In contrast, the present invention, in this preferred embodiment, relies on two thermally assisted separation steps: a first stage, filtration or compression depending on the dehydrated material, at low pressure (of the order of 3 bar in a preferred embodiment) followed by a separation step at higher pressure, the piston temperature remains constant.

Dans un tel procĆ©dĆ© selon l'invention, la premiĆØre Ć©tape permet de sĆ©parer Ć  moindre coĆ»t une grande quantitĆ© de liquide. Pendant la seconde phase de sĆ©paration, un gain de siccitĆ© important peut ĆŖtre espĆ©rĆ©, selon les produits dĆ©shydratĆ©s, mĆŖme Ć  faible pression (de l'ordre de 7 bars). Par ailleurs, la sĆ©paration est plus rapide qu'Ć  tempĆ©rature ambiante.In such a method according to the invention, the first step makes it possible to separate a large quantity of liquid at a lower cost. During the second phase of separation, a significant increase in dryness can be expected, depending on the dehydrated products, even at low pressure (of the order of 7 bars). Moreover, the separation is faster than at room temperature.

Pour passer Ć  un procĆ©dĆ© en continu, compte tenu des pressions Ć  mettre en oeuvre, la technologie de la presse Ć  vis peut ĆŖtre utilisĆ©e dans la prĆ©sente invention. Comme dĆ©jĆ  Ć©voquĆ© plus haut, il est possible de chauffer non seulement les piĆØces exerƧant une pression mais Ć©galement les autres parois en contact avec le produit Ć  dĆ©shydrater. Ce chauffage peut ĆŖtre rĆ©alisĆ© Ć  l'aide de rĆ©sistances Ć©lectriques mais Ć©galement en utilisant un fluide caloporteur (huile thermique, eau chaude, vapeur, air chaud, buĆ©es issues d'un sĆ©cheur...).To proceed to a continuous process, given the pressures to be implemented, the technology of the screw press can be used in the present invention. As already mentioned above, it is possible to heat not only the parts exerting pressure but also the other walls in contact with the product to be dehydrated. This heating can be achieved using electrical resistances but also by using a coolant (thermal oil, hot water, steam, hot air, steam from a dryer ...).

La prĆ©sente invention ne se limite pas aux modes de rĆ©alisation dĆ©crits ci-dessus Ć  titre d'exemples non limitatifs et aux variantes Ć©voquĆ©es. Elle concerne Ć©galement les autres variantes et applications Ć  la portĆ©e de l'homme du mĆ©tier dans le cadre des revendications ci-aprĆØs.The present invention is not limited to the embodiments described above by way of non-limiting examples and the variants mentioned. It also relates to other variants and applications within the scope of the skilled person within the scope of the claims below.

Claims (12)

  1. A method of thermally assisted mechanical dehydration in which a product to dehydrate is introduced into a filtration and/or compression device, in which a provision of heat is supplied, and which comprises a first step at a first pressure of less than 7 bars during which the product to dehydrate is heated to a temperature less than the evaporation temperature of the liquid to eliminate and the liquid to eliminate is progressively collected,
    characterized in that this first step is of a duration comprised between 5 minutes and several hours, and in that this first step at a first pressure is followed by a second step at a second pressure, this second pressure being greater than the first pressure and less than 30 bars.
  2. A method according to claim 1, characterized in that the first pressure is comprised between 1.5 and 4 bars.
  3. A method according to one of claims 1 or 2, characterized in that the filtration and/or compression device comprises a chamber (2, 4) having a wall at least part of which is heated, and in that the product to dehydrate is heated by conduction from the heated part of the wall.
  4. A method according to claims 1 to 3, characterized in that the second step is carried out at a lower temperature than the evaporation temperature of the liquid to extract.
  5. A method according to claims 3 and 4, characterized in that in the second step the heated part of the wall remains at a substantially constant temperature, that temperature corresponding to the temperature of said heated part of the wall in the filtration and/or compression device at the end of the first compression step.
  6. A method according to one of claims 3 or 5, characterized in that the liquid to eliminate mainly contains water, and in that the heated part of the wall is brought to a temperature comprised between 40Ā°C and 90Ā°C in the first step.
  7. A method according to one of claims 1 to 5, characterized in that it comprises before the first step a dehydration step at ambient temperature, without provision of heat, at a pressure corresponding to the first pressure and during which the liquid to eliminate is progressively collected.
  8. A method according to one of claims 1 to 7, characterized in that it is applied to the pretreatment of a moist biomass, excluding wood.
  9. A method according to claim 8, characterized in that the moist biomass undergoes a final step of thermal drying in a dryer, in that the dryer is provided with a heat exchanger at the output, and in that the energy of the vapors collected in the heat exchanger is at least partially used to perform heating during the preceding steps of the method.
  10. A method according to one of claims 1 to 7, characterized in that it is applied to the dehydration of liquid or pasty waste, excluding residual municipal sludge and drinking water sludge.
  11. A method according to one of claims 1 to 7, characterized in that it is applied to the extraction of green juice from a moist biomass, excluding wood.
  12. A method according to claim 11, characterized in that the temperature of the heated wall remains below 60Ā°C.
EP08871924.0A 2007-11-12 2008-11-10 Method for mechanical dehydration with thermal assistance Not-in-force EP2212637B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0707911A FR2923587B1 (en) 2007-11-12 2007-11-12 THERMALLY ASSISTED MECHANICAL DEHYDRATION METHOD
PCT/FR2008/001586 WO2009095556A2 (en) 2007-11-12 2008-11-10 Method for mechanical dehydration with thermal assistance

Publications (2)

Publication Number Publication Date
EP2212637A2 EP2212637A2 (en) 2010-08-04
EP2212637B1 true EP2212637B1 (en) 2013-05-01

Family

ID=39577716

Family Applications (1)

Application Number Title Priority Date Filing Date
EP08871924.0A Not-in-force EP2212637B1 (en) 2007-11-12 2008-11-10 Method for mechanical dehydration with thermal assistance

Country Status (4)

Country Link
EP (1) EP2212637B1 (en)
ES (1) ES2423306T3 (en)
FR (1) FR2923587B1 (en)
WO (1) WO2009095556A2 (en)

Family Cites Families (9)

* Cited by examiner, ā€  Cited by third party
Publication number Priority date Publication date Assignee Title
GB609768A (en) * 1946-03-21 1948-10-06 Charles Goodall Improvements relating to grass or like drying apparatus
FR1032870A (en) * 1951-02-19 1953-07-06 Method and device for spraying and drying cut grass and other vegetable matter
FR2425043A1 (en) * 1978-05-03 1979-11-30 Gourmelen Jacqueline Vegetable crop drying system - uses two-stage action, with predrying air warmed using waste heat from drying plant
US4380496A (en) * 1979-03-22 1983-04-19 Uop Inc. Mechanical dewatering process utilizing a nonuniform screw conveyor
FR2601380B1 (en) * 1986-07-08 1989-08-18 Clextral PROCESS AND DEVICE FOR THE CONTINUOUS MANUFACTURE OF MIXED FUELS BASED ON ORGANIC MATERIALS AND HYDROCARBON MATERIALS
AT398389B (en) * 1992-11-06 1994-11-25 Andritz Patentverwaltung METHOD AND SYSTEM FOR SEPARATING SOLID / LIQUID MIXTURES
FR2748685B1 (en) * 1996-05-14 1998-08-14 Clextral METHOD AND INSTALLATION FOR CONTINUOUS EXTRACTION OF A LIQUID CONTAINED IN A RAW MATERIAL
US6076279A (en) * 1998-01-09 2000-06-20 Finbark Oy Method and a device for improving liquid removal
DE19860181C1 (en) * 1998-12-24 2000-06-29 A & U Abfallwirtschaft & Umwel Water removal from contaminated residues in concrete pans heated at the base and covered by a semipermeable membrane.

Also Published As

Publication number Publication date
EP2212637A2 (en) 2010-08-04
WO2009095556A2 (en) 2009-08-06
FR2923587B1 (en) 2017-10-20
ES2423306T3 (en) 2013-09-19
WO2009095556A3 (en) 2009-09-24
FR2923587A1 (en) 2009-05-15

Similar Documents

Publication Publication Date Title
CA2723116C (en) Method, device and use of a device for producing fuel from moist biomass
EP3484945B1 (en) Method for treating lignocellulosic biomass by impregnation and steam explosion
EP3287418B1 (en) Method for ultra-dehydration of thickened or pasty products forming biomass and facility for implementing the method
FR2461752A1 (en) FERMENTATION PROCESS FOR THE PRODUCTION OF ETHANOL OR SIMILAR VOLATILE ORGANIC COMPOUND
FR2574810A1 (en) MULTIPLE SOIL REACTOR AND METHOD OF HEAT TREATING CARBONACEOUS MATERIALS
FR3087790A1 (en) PROCESS FOR THE CONTINUOUS MANUFACTURE OF A FUEL MATERIAL FOR INDUSTRIAL BOILER, MATERIAL AND CORRESPONDING INSTALLATION
CA3047963A1 (en) Ligno cellulosic biomass treatment process
EP0243243A2 (en) Process and apparatus for separating constituent parts from a suspension
CN103124792A (en) A process for the conversion of biomass of plant origen, and a combustion process
EP2212637B1 (en) Method for mechanical dehydration with thermal assistance
US20050142265A1 (en) Preservation of sugar cane and other plant materials
CN105712897A (en) Tea polyphenol extracting and recycling method
BE1001794A6 (en) Flour recovery process and oil from fish waste.
FR2601118A1 (en) PROCESS FOR DRYING PLANT MATERIALS WITH HIGH PRESSURE STEAM
WO2006024762A1 (en) Reduced-pressure cooling method and installation for implementing same
WO2018095989A1 (en) Method for manufacturing pellets which comprises recovering steam from the grinding of biomass, and associated facility
WO1984000475A1 (en) Method for the dehydration of wet plants
FR2960870A1 (en) Drying pasty materials such as sludge from treatment plants, comprises subjecting sludge exiting from electrode hydration to laying operation that is moderated to preserve structure of sludge present in outlet of electro dehydration
RO120915B1 (en) Process for dewatering raw brown coal
EP0819156A1 (en) Method and device for producing fuel by continuously pyrolysing crushed or pasty waste
FR2509025A1 (en) PROCESS FOR THE DRYING OF A WET MATERIAL CONTAINING SOLUBLE SALTS, IN PARTICULAR POTASSIA SALT, AS WELL AS DEVICE FOR CARRYING OUT THIS PROCESS
RU2281322C2 (en) Distillery dregs dehydration line and distillery dregs dehydration process
EP4347749A1 (en) Stepwise method for continuously producing a combustible material by explosive decompression
FR2774926A1 (en) Dewatering solid-liquid matrices such as sludges
FR3115538A1 (en) Process for treating lignocellulosic biomass

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20100517

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MT NL NO PL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: AL BA MK RS

RIN1 Information on inventor provided before grant (corrected)

Inventor name: AUDUC, BERNARD

Inventor name: MAHMOUD, AKRAMA

Inventor name: FERNANDEZ, MARIA AURORA

Inventor name: ARLABOSSE, PATRICIA

DAX Request for extension of the european patent (deleted)
GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: ECOLE NATIONALE SUPERIEURE DES TECHNIQUES INDUSTRI

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: ECOLE NATIONALE SUPERIEURE DES MINES D'ALBI-CARMAU

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: ECOLE NATIONALE SUPERIEURE DES MINES D'ALBI-CARMAU

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MT NL NO PL PT RO SE SI SK TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: AT

Ref legal event code: REF

Ref document number: 610192

Country of ref document: AT

Kind code of ref document: T

Effective date: 20130515

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: FRENCH

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602008024348

Country of ref document: DE

Effective date: 20130627

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK05

Ref document number: 610192

Country of ref document: AT

Kind code of ref document: T

Effective date: 20130501

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2423306

Country of ref document: ES

Kind code of ref document: T3

Effective date: 20130919

REG Reference to a national code

Ref country code: NL

Ref legal event code: VDEP

Effective date: 20130501

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130902

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130802

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130901

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130801

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130801

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20140204

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602008024348

Country of ref document: DE

Effective date: 20140204

BERE Be: lapsed

Owner name: ECOLE NATIONALE SUPERIEURE DES MINES D'ALBI-CARMA

Effective date: 20131130

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20131110

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20131130

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20131130

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20131130

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20131110

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20131110

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20081110

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20130501

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 8

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 9

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20210922

Year of fee payment: 14

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20211203

Year of fee payment: 14

Ref country code: IE

Payment date: 20211122

Year of fee payment: 14

Ref country code: DE

Payment date: 20211110

Year of fee payment: 14

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 602008024348

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20221110

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20230601

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20221130

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20231228

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20221111

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20221111