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WO2018050941A1 - Multi-bed pilot plant and process for biomass fractionation - Google Patents

Multi-bed pilot plant and process for biomass fractionation Download PDF

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Publication number
WO2018050941A1
WO2018050941A1 PCT/ES2017/070611 ES2017070611W WO2018050941A1 WO 2018050941 A1 WO2018050941 A1 WO 2018050941A1 ES 2017070611 W ES2017070611 W ES 2017070611W WO 2018050941 A1 WO2018050941 A1 WO 2018050941A1
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WO
WIPO (PCT)
Prior art keywords
reactors
liquid fluid
biomass
pilot plant
reactor
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/ES2017/070611
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Spanish (es)
French (fr)
Inventor
Gianluca GALLINA
Juan GARCÍA SERNA
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Universidad de Valladolid
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Universidad de Valladolid
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Application filed by Universidad de Valladolid filed Critical Universidad de Valladolid
Publication of WO2018050941A1 publication Critical patent/WO2018050941A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H8/00—Macromolecular compounds derived from lignocellulosic materials

Definitions

  • the present invention refers to a multilevel pilot process and plant for fractionation of biomass, where soluble compounds of the residual and non-residual biomass are continuously extracted and fractionated, using water as a solvent. or water with a low concentration of acid or base; or other fluids.
  • the plant of the invention allows ease and speed in operation by rapid exchange of the exhausted solid without stopping the process. It also allows rapid operation through a series process without disassembling some reactors from the pilot plant at the end of the experiments. It is also emphasized that the plant of the invention allows to operate with different types of biomass, without limitations due to the size of the biomass particles, also allowing the exhausted solid to be collected entirely. Finally, it is emphasized that the innovations of the invention manage to greatly reduce the time of the extraction process and also manage to eliminate downtimes.
  • lignocellulosic materials belong to second generation raw materials, and can be obtained from various sources, such as wood waste, agricultural or municipal waste; that do not interfere with crops for direct human consumption. They consist mainly of lignin, cellulose and hemicellulose, associated in a resistant structure, whose rupture requires a considerable amount of energy. However, thanks to their differentiated composition, they allow to obtain fuels and multiple high-value chemicals.
  • hydrothermal hydrolysis A promising, clean and cheap way to depolymerize hemicellulose in monosaccharides is the process called hydrothermal hydrolysis, which simply consists of treating the biomass with water with different temperatures, or with water with a low acid concentration.
  • Patent with publication number WO 2015009986 A2 describes a method for obtaining hemicellulose using water or water with acid, through a flow reactor.
  • Patent No. Publication WO 201 1091044 A1 describes a process for extracting cellulose and hemicellulose from biomass, with subcritical and supercritical water, through a continuous reactor fed with a suspension of water and biomass.
  • the patent with publication number US 6228177 B1 describes a series system, for the extraction of lignocellulosic material, in which the reactors are cooled by immersion in cold water.
  • the invention proposes a multi-pilot pilot plant for biomass fractionation which aims to continuously extract and fractionate bioproducts such as polyphenols, betaglucans, caffeine and biopolymers such as hemicellulose, from residual and non-residual lignocellulosic biomass from different sources.
  • Vegetable biomass contains many interesting products. Some of these, such as the polyphenols contained in the seeds and skins of grapes, the beta-glucans contained in oats, barley and mushrooms, and especially hemicellulose, an essential component of plants, and that appear in all products of plant origin, can be extracted only with water with different temperatures.
  • the first two compounds mentioned are of great importance in human health and well-being: polyphenols are compounds with antioxidant capacity that have aroused great interest in health and in the prevention of diseases associated with an increase in cellular oxidation processes (cancer , cardiovascular diseases and neurodegenerative diseases); betaglucans improve blood glucose control, as well as lipid levels such as cholesterol or triglycerides.
  • Hemicellulose when isolated from biomass in molecular masses above 3-5 kDa, has unique properties. It can be used to produce films for packaging applications instead of synthetic plastics, it works as barriers against oxygen penetration; Another important application is the production of aerogels to isolate food products.
  • Xylose from hemicellulose can be converted into furfural, which is a precursor used in different fields, such as petroleum refining, plastics, pharmaceuticals and agrochemicals.
  • furfural is a precursor used in different fields, such as petroleum refining, plastics, pharmaceuticals and agrochemicals.
  • Xylose can also be hydrogenated or enzymatically transformed into xylitol, which is a sweetening agent and is also used for the prevention of tooth decay.
  • First generation products are manufactured from edible biomass such as starch-rich or oily plants; second generation products use biomass that It consists of the residual inedible parts of current crops or other non-food sources, such as perennial herbs or algae. These are widely recognized as having significantly greater potential to replace fossil products (King, 2010).
  • Lignocellulosic materials belong to second-generation raw materials, and can be obtained from various sources, such as wood waste, agricultural or municipal waste, which do not interfere with crops for direct human consumption. They consist mainly of lignin, cellulose and hemicellulose, associated in a resistant structure, whose rupture requires a considerable amount of energy; However, thanks to their differentiated composition, they allow to obtain fuels and multiple high-value chemicals.
  • Lignocellulosic biomass can be divided into cellulose, hemicellulose and lignin, from which sugars, fuels, materials and chemicals can be produced. Energy can be produced from processing waste.
  • the plant of the invention offers great improvements in the extraction of hemicellulose, an integral part of the biorefinery process.
  • the plant of the invention includes numerous innovations for the extraction of bioproducts from biomass, and allows:
  • the multi-strand pilot plant is applicable to the soluble coffee processing industries; however, in these industries the vacuum extractor is simply used, since tubular structures that include said industries are large enough to dislodge the exhausted solid. On the other hand, at the pilot plant level the solid material gets stuck and creates serious problems to make a continuous extraction operation possible.
  • the plant of the invention is able to load the biomass into cartridges that are inserted hot in each reactor, so that a series of valves manage to isolate the beds so that the exhausted biomass can be exchanged without stopping the fractionation and extraction process achieved in the plant of the invention.
  • the multi-strand pilot plant of the invention comprises reactors interconnected with each other by a pipe circuit through which a liquid fluid flows driven by at least one motorcycle pump; where the reactors include biomass container cartridges, a liquid fluid inlet that runs through the biomass contained within the cartridges and a liquid fluid outlet that contains various substances extracted from the biomass housed inside the cartridges.
  • the pilot plant of the invention further comprises reactors in vertical arrangement that have the liquid fluid inlet above the cartridge, and the liquid fluid outlet is located in a lower part of the reactors.
  • At the lower ends of the reactors connect opening and closing devices of said reactors located below the cartridges; where the cartridges are introduced into the reactors and are removed from the interior of said reactors through the opening and closing devices when they are placed in an open position.
  • the piping circuit comprises a part of the flow through which the liquid fluid directed towards the liquid fluid inlets flows into the reactors, and some return parts through which the liquid fluid flows when it leaves the reactors; where in said parts of the piping circuit, valves are inserted that allow the isolation of the reactors for the exchange of cartridges without stopping the operation of the pilot plant.
  • Each of the outlets of the pipeline circuit includes a first three-way valve and a second two-way valve interspersed in a branch that starts from the inlet to the reactor.
  • Each of the return parts of the pipeline circuit includes at least a first two-way valve.
  • An outlet of the first three-way valve connects to a section of pipe that feeds the reactor; while another outlet of the first three-way valve feeds an intermediate section that connects with another first three-way valve interspersed in another one-way part of the pipeline circuit.
  • the first two-way valve is interspersed in a pipe section that starts from the reactor outlet and connects to said intermediate section.
  • the plant of the invention includes a two-position needle valve interspersed in an end section of pipe that connects to the pipe section of the reactor outlet and with a heat exchanger that connects to a second three-way valve that has a outlet that connects with a first tube to take samples of the liquid fluid, and a second outlet that connects with a second tube.
  • An initial section of the pipe circuit includes initial heat exchangers in combination with a main heater located after said initial heat exchangers.
  • the multileight pilot plant comprises a back pressure valve to regulate the pressure inside the reactors; wherein said backpressure valve is located in an initial branch of the first part of the pipeline circuit.
  • the return part of a last reactor corresponding to the liquid fluid outlet of said last reactor connects with a feedback bypass leading to an initial area of the first part of the pipe circuit.
  • Each of the reactors has an additional upper outlet where it connects a pipe bypass that flows into a container; where in said pipe bypass a third two-way valve is inserted.
  • each of the reactors opening and closing devices comprises a ball valve.
  • the pilot plant comprises parachute devices fixed to the opening and closing devices located at the lower ends of the reactors; where sayings Parachute devices dampen the fall of the cartridges when removed from inside the reactors.
  • the reactors are homogeneously coated by wrapping resistors to heat said reactors and maintain the temperature.
  • Each of the reactors of the plant comprises:
  • an inner tubular housing having a perforated lower base and an open upper base; where the tubular mesh is located within said inner tubular housing.
  • the tubular mesh comprises two removable half parts that are coupled to each other through two opposite generatrices that follow a broken path.
  • the inner tubular housing comprises two separate parts: a first part that includes the perforated lower base, and a second part that includes a narrowing where the open upper base is located.
  • the outer tubular casing of each reactor comprises a main body and a cover that closes the main body at its upper end, while its lower end connects to the opening and closing device; where the cover includes a liquid fluid inlet into the reactor; and where the main body includes a liquid fluid outlet and the additional outlet that connects to the pipe bypass that drains part of the liquid fluid into the container.
  • the tubular mesh, lower tubular casing and outer tubular casing have a cylindrical configuration and consist of a metallic material.
  • Each heat exchanger located in the return part of the pipe circuit comprises two concentric tubes: exterior and interior; where the liquid fluid contained in the reactor is cooled from the inner tube, cooled by water flowing through the outer tube.
  • Each of the parachute devices comprises a front plate that hangs at least two suspension elements connected to a part of the opening and closing device; wherein said faceplate is located below the opening and closing device to receive the cartridge when said opening and closing device is opened.
  • the pilot plant comprises a first moto-pump that is used at the beginning of the process to fill the reactors before the pipeline circuit is opened to carry out the continuous extraction and fractionation process of the soluble compounds of the residual biomass and not residual Said first moto-pump is fed by a clean liquid fluid or not, contained within a first tank.
  • the pilot plant also comprises a second motorcycle pump that drives the liquid fluid through the pipeline circuit to carry out the continuous extraction and fractionation process of the soluble compounds of the residual and non-residual biomass.
  • Said second motor-pump is fed by a liquid fluid contained within a second reservoir.
  • the process comprises an additional phase in which the liquid fluid extracted from the last reactor is returned to the initial part of the pipeline circuit.
  • Figure 1 Shows a view of the multileight pilot plant for biomass fractionation, object of the invention. It comprises a set of reactors in combination with other elements to carry out the extraction and continuous fractionation of soluble compounds. The process for carrying out the fractionation of biomass is also an object of the invention.
  • Figure 2. Shows a view of a part of the plant of the invention.
  • Figure 3. Shows an exploded view of one of the reactors together with a ball valve, which is part of the plant of the invention.
  • Figure 4.- Shows a sectional view of the reactor.
  • Figure 5. Shows a plan view of one of the reactor parts.
  • the multileight pilot plant for biomass fractionation comprises several reactors 1 in vertical arrangement interconnected with each other by means of one-way parts through which a liquid fluid runs towards some liquid fluid inlets of the reactors 1, and return parts through which the liquid fluid flows when it leaves the reactors 1; where each of the reactors works in series with the others, with the possibility of being able to exclude one reactor 1 from the others; and where said return and return parts are part of a pipe circuit through which liquid fluid flows.
  • Each of the reactors 1 comprises:
  • tubular metal mesh 2 formed by two removable half parts 2a, 2b that are coupled to each other through two opposite generatrices that follow a broken path; where said tubular mesh 2 is filled with biomass.
  • an inner tubular housing 3 made of stainless steel with a perforated bottom base 4 and a upper base open 5; wherein within said inner tubular housing 3 the tubular mesh 2 is located; and wherein said inner tubular housing 3 comprises two separate parts: a first part 3a that includes the perforated lower base 4 and a second part 3b that includes a narrowing 6 where the open upper base 5 is located.
  • Said outer tubular casing 7 comprises a main body 7a and a cover 7b which closes the main body 7a by its upper end, while its lower end connects with a ball valve 9.
  • the tubular mesh 2, lower tubular housing 3 and outer tubular housing 7 have a cylindrical configuration.
  • the cartridge assembly is inserted from below into the outer tubular casing 7 through the ball valve 9 when it is in the open position until it is fully inserted into said outer tubular casing 7.
  • the ball valve 9 closes and when the extraction is finished by passing a liquid fluid through the interior of the reactor 1, the ball valve 9 is opened by dropping down the gravity of the cartridge that is drawn outwards. , so that the outlet of the cartridge is damped by a parachute device 10 located in the outlet area of the ball valve 9.
  • a constant flow of water enters through an inlet opening 1 1 located at the top of each reactor 1 making a downward path through the interior of said reactor 1 until it exits through an outlet port 12 located at the bottom of the reactor 1; where the inlet 11 is located in the cover 7b of the outer tubular casing 7 and the outlet 12 is located in a lower part of the main body 7a of said outer tubular casing 7.
  • the liquid outflow can go to the next reactor 1, or it can be diverted in order to exclude the next reactor 1, and move on to the next reactor 1.
  • the biomass can be discharged (through the opening of the ball valve 9 and the rapid removal of the cartridge ) of the reactor 1 in which the extraction process is completed, and another reactor 1 can be loaded with another cartridge, then divert in that reactor 1 the liquid flow to continue with the extraction process.
  • the plant of the invention allows operation Fast and continuous without stops.
  • Another important feature of the plant of the invention is the adjustment of water temperature and energy control. To do this, before entering the reactors 1, the water passes through a main heater 13 formed by a spiral coil wound around a solid metal body; where said spiral coil is covered by an electric clamp resistor.
  • the water then enters the reactors 1, which are homogeneously coated with clamp wraps 14. After leaving the reactor 1, the liquid fluid enters a heat exchanger 15 of concentric tubes. On the outside, the water supply of the plant flows, which is previously heated through initial heat exchangers 16 and then passes to the main heater 13 described above. The entire system is thermally insulated with a layer of glass wool covered with aluminum foil. The total heat savings is 85% and the cooling savings are close to 100%.
  • Each reactor 1 can be emptied of the pressurized hot liquid fluid before removing the cartridge constituted by the tubular mesh 2 and inner tubular casing 3. Between each pair of adjacent reactors 1 is located the heat exchanger 15 with concentric tubes: outer and inner; where the liquid contained in the reactor 1, cooled by water flowing through the outer tube, is discharged from the inner tube. These heat exchangers 15 also allow the sampling of liquid from each reactor during the reaction of the liquid fluid with the biomass.
  • the plant also includes safety valves in each reactor 1 that avoid any overpressure. Also included is a thermostat that prevents overheating of the solid metal body of the main heater 13.
  • the liquid contained in the reactor 1 is discharged from the inner tube after the extraction operation, and cold water flows through the outer tube which then feeds the plant of the invention.
  • the biomass is introduced into the tubular mesh 2, which can be opened longitudinally, and inserted between the two parts 3a, 3b of the inner tubular casing 3.
  • the first part 3a is open at the upper end and at the lower end it has the perforated lower base 4 with holes with a diameter between 5 mm and 0.5 mm.
  • the assembly of the tubular mesh 2 and the inner tubular casing 3 is inserted, through the ball valve 9, into the outer tubular casing 7 closed by the upper end by the cover 8 which is It can be removed if reactor 1 becomes clogged.
  • the size of the biomass particles loaded in the reactor 1 has to be larger than the diameter of the holes of the perforated bottom base 4 of the inner tubular casing 3, which functions as a filter preventing solid biomass from being removed from the bed and dragged through the different elements of the plant of the invention.
  • the plant of the invention comprises an operating unit of reactor 1 where the process for biomass fractionation is carried out.
  • FIG 1 a plant is shown that includes several connected reactor units, which can operate in series with one another, or separately, and where also carries out the process for the fractionation of biomass.
  • the cartridge is pushed until it enters completely, and then the ball valve 9 located below the cartridge is closed. At this time, the reactor 1 is filled with water, driven by a first motor pump 19, making sure that the liquid enters the reactor 1 and does not leak through the pipeline circuit.
  • each reactor 1 is isolated from the rest of the pilot plant system by closing a first two-way valve 20 and a second needle valve 21 located at the exit of each reactor 1.
  • a second valve is also opened 22 two-way and a first three-way valve 23 is moved, such that water enters only in a reactor 1, and in the tube segment between the reactor and said first three-way valve 23.
  • the first three-way valve 23 can divert the flow to the next reactor 1 or to the next first three-way valve 23, avoiding the previous reactor 1.
  • the reactor 1 is heated homogeneously by the wrapping resistors 14 to a temperature slightly below the minimum temperature needed to begin the extraction of the compound to be extracted.
  • Hemicellulose begins to be extracted at temperatures above 100 ° C; so that if it is decided to extract said hemicellulose compound, the reactor 1 must be preheated and wait for the reactor 1 to reach temperatures above 100 ° C.
  • a second motorcycle pump 27 is activated to drive the flow of liquid that previously passes through the initial heat exchangers 16, functioning as a cooling liquid of another hot liquid leaving the system, and at the same time achieving a first preheating . Consequently, it achieves further preheating, by means of the main heater 13, towards a temperature higher than the one required to operate; following the liquid fluid then to the first three-way valve 23.
  • said first three-way valve 23 is still placed in a position where the flow of liquid is diverted to the next first three-way valve 23, and not to the reactor 1.
  • the reactor temperature is raised to the conditions under which it is desired to operate; the first three-way valve 23 being adjusted, so that the flow of liquid enters the reactor 1, and at the same time the first two-way valve 20 is opened so that the liquid can leave the reactor 1.
  • the extraction of the soluble compounds from the biomass in the reactor 1 the liquid flow enters the reactor 1, passes through the biomass bed, extracts the soluble compounds, and leaves the reactor.
  • the flow of liquid leaving the reactor 1 reaches another first three-way valve 23, so that by acting on this first three-way valve 23, the flow can be directed to the next reactor 1 or to the next first three-way valve 23 .
  • This operation can be repeated for each reactor unit in the pilot plant system. In this way, each reactor 1 can be integrated into the extraction process, or it can be omitted.
  • the hot liquid stream is returned and enters the inside of the initial heat exchangers 16 transferring heat to the liquid fed into the system.
  • the liquid outlet therefore, cools, and depressurizes through the back pressure valve 17, and finally exits the system.
  • the back pressure valve 17 regulates the pressure of the entire extraction system, so that when it is desired to interrupt the reaction in a reactor 1, the flow of liquid is diverted, blocking the supply to the corresponding reactor unit 1 to be isolated from the system.
  • the first three-way valve 23 that precedes the respective reactor 1 is rotated and the first two-way valve 20 placed at the exit of said reactor 1 is closed, thus excluding the corresponding reactor 1 from the system.
  • the liquid flow can be directed to the subsequent reactor unit 1 (loaded with a biomass cartridge, as explained above), or it can be directed to the next three-way first valve 23, which in turn can direct the flow.
  • the needle valve 21 has an outlet that flows into the heat exchanger 15, so that when said needle valve 21 is opened, the liquid contained in the reactor 1 passes to the heat exchanger 15 and is cooled by another flowing liquid on the outside of the heat exchanger 15. In this way, the pressurized liquid contained within the reactor does not vaporize during the opening of the needle valve 15, and exits as a normal liquid without pressure.
  • This pilot plant system allows to completely empty each reactor of the liquid, once the extraction process is completed.
  • a second three-way valve 28 is connected which allows the liquid to be directed to a shorter first tube 29 to take a sample of the product, or to a second longer tube 30 connected to a system Drain
  • the ball valve 9 is opened below the reactor 1, causing the cartridge containing the exhausted biomass to fall into the parachute device 10.
  • the cartridge can be removed and open, so that the bad tubular 2 is removed from the inside of the inner tubular housing 3 and subsequently the tubular mesh 2 is opened longitudinally, so that all the biomass can be collected in a solid state.
  • another cartridge Fresh biomass container can be quickly reloaded, restarting the extraction process in the new mounted cartridge.
  • the first motor pump 19 is used at the beginning of the process to fill the reactors 1 before the pipeline circuit is opened to carry out the process of continuous extraction and fractionation of the soluble compounds of the residual and non-residual biomass. Said first motor pump 19 is fed by a clean or not liquid fluid, contained within a first tank 31.
  • the second motor pump 27 drives the liquid fluid through the piping circuit to carry out the process of continuous extraction and fractionation of the soluble compounds of the residual and non-residual biomass. Said second motor pump 27 is fed with a liquid fluid contained within a second tank 32.
  • the two motor pumps 19, 27 are fed independently of liquid fluids contained within the tanks 31, 32; that in one embodiment of the invention said liquid fluids are water.
  • Each of the parachute devices 10 comprises a metal faceplate 10a that hangs on two suspension elements 10b connected to a part of the ball valve 9; wherein said faceplate 10a is located below said ball valve 9.
  • the suspension elements 10b comprise chains and in another embodiment comprise for example braces.

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  • Organic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention relates to a multi-bed pilot plant comprising vertically arranged reactors (1) that have the liquid fluid inlet arranged above biomass-containing cartridges, and a liquid fluid outlet arranged in a lower part of the reactors. Devices for opening and closing said reactors are connected on the lower ends of the reactors, below the cartridges, the cartridges being independently inserted into the reactors and extracted from the inside of said reactors through the opening and closing devices when they are in an open position, while maintaining the operation of the plant. The reactors can also be independently isolated in order to replace cartridges as required, without stopping the operation of the pilot plant.

Description

PROCESO Y PLANTA PILOTO MULTILECHO PARA FRACCIONAMIENTO DE BIOMASA  PROCESS AND PLANT PULOT MULTILECHO FOR FRACTIONATION OF BIOMASS

DESCRIPCIÓN Objeto de la invención DESCRIPTION Object of the invention

La presente invención, según se expresa en el enunciado de esta memoria descriptiva, se refiere a un proceso y planta piloto multilecho para fraccionamiento de biomasa, donde se extraen y fraccionan en continuo compuestos solubles de la biomasa residual y no residual, utilizando como solvente agua o agua con una baja concentración de ácido o base; u otros fluidos. La planta de la invención permite facilidad y velocidad en la operación mediante un intercambio rápido del sólido exhausto sin detener el proceso. Permite además operar con rapidez mediante un proceso en serie sin desmontar unos reactores de la planta piloto al final de los experimentos. Se destaca también que la planta de la invención permite operar con diferentes tipos de biomasa, sin limitaciones debidas al tamaño de las partículas de la biomasa, permitiendo también recolectar enteramente el sólido exhausto. Por último se destaca que las innovaciones de la invención consiguen reducir en gran medida el tiempo del proceso de extracción y también consiguen eliminar los tiempos de parada.  The present invention, as expressed in the statement of this specification, refers to a multilevel pilot process and plant for fractionation of biomass, where soluble compounds of the residual and non-residual biomass are continuously extracted and fractionated, using water as a solvent. or water with a low concentration of acid or base; or other fluids. The plant of the invention allows ease and speed in operation by rapid exchange of the exhausted solid without stopping the process. It also allows rapid operation through a series process without disassembling some reactors from the pilot plant at the end of the experiments. It is also emphasized that the plant of the invention allows to operate with different types of biomass, without limitations due to the size of the biomass particles, also allowing the exhausted solid to be collected entirely. Finally, it is emphasized that the innovations of the invention manage to greatly reduce the time of the extraction process and also manage to eliminate downtimes.

Problema técnico a resolver y antecedentes de la invención Technical problem to solve and background of the invention

En la actualidad, los materiales lignocelulósicos pertenecen a las materias primas de segunda generación, y se pueden obtener de varias fuentes, tales como residuos de madera, residuos agrícolas o municipales; que no interfieren con los cultivos para el consumo humano directo. Se componen principalmente de lignina, celulosa y hemicelulosa, asociadas en una estructura resistente, cuya ruptura requiere una cantidad considerable de energía. Sin embargo, gracias a su composición diferenciada, permiten obtener combustibles y múltiples productos químicos de alto valor. Currently, lignocellulosic materials belong to second generation raw materials, and can be obtained from various sources, such as wood waste, agricultural or municipal waste; that do not interfere with crops for direct human consumption. They consist mainly of lignin, cellulose and hemicellulose, associated in a resistant structure, whose rupture requires a considerable amount of energy. However, thanks to their differentiated composition, they allow to obtain fuels and multiple high-value chemicals.

Una forma prometedora, limpia y barata para despolimerizar la hemicelulosa en monosacáridos es el proceso llamado hidrólisis hidrotermal, que simplemente consiste en el tratamiento de la biomasa con agua con diferentes temperaturas, o con agua con una baja concentración de ácido. A promising, clean and cheap way to depolymerize hemicellulose in monosaccharides is the process called hydrothermal hydrolysis, which simply consists of treating the biomass with water with different temperatures, or with water with a low acid concentration.

La forma más eficiente para extraer la hemicelulosa de la biomasa es el uso de sistemas en el flujo, en el que unos reactores se cargan con pellets o polvo de biomasa, mientras que un flujo continuo de líquido (agua o agua con ácido) se introduce continuamente en los reactores, extrayendo e hidrolizando la hemicelulosa. Para asegurarse de que el sistema sea eficiente, es necesario que el ratio entre la biomasa y el agua sea alto, a fin de obtener un producto concentrado. Uno de los principales problemas de las instalaciones actualmente existentes para la finalidad descrita, es cargar y descargar el material sólido contenido en cada reactor una vez que se haya completado el proceso de extracción. De hecho, la biomasa húmeda se hincha y se compacta, lo que hace imposible su remoción sin parar el sistema, y sin abrirlo. Esto implica tiempos de inactividad largos. En muchos casos se utilizan partículas con dimensiones del orden de mieras, que presuponen la trituración de la biomasa, con el consiguiente consumo de energía, y el bombeo de la suspensión constituida de agua y biomasa, lo que también supone un consumo de energía añadido. The most efficient way to extract hemicellulose from biomass is the use of systems in the flow, in which some reactors are loaded with pellets or biomass powder, while a continuous flow of liquid (water or water with acid) is introduced continuously in the reactors, extracting and hydrolyzing hemicellulose. To ensure that the system is efficient, it is necessary that the ratio between biomass and water is high, in order to obtain a concentrated product. One of the main problems of the facilities currently existing for the purpose described, is to load and unload the solid material contained in each reactor once the extraction process has been completed. In fact, wet biomass swells and compacts, which makes removal impossible without stopping the system, and without opening it. This implies long downtimes. In many cases particles with dimensions of the order of microns are used, which presuppose the crushing of the biomass, with the consequent energy consumption, and the pumping of the suspension constituted of water and biomass, which also implies an added energy consumption.

La patente con n° de publicación WO 2015009986 A2 describe un método para la obtención de hemicelulosa utilizando agua o agua con ácido, a través de un reactor en flujo. Patent with publication number WO 2015009986 A2 describes a method for obtaining hemicellulose using water or water with acid, through a flow reactor.

La patente con n° de publicación US 6022419 A se refiere a un reactor en el que el volumen ocupado por el sólido (serrín), disminuye continuamente por efecto de un muelle, que lo empuja hacia una extremidad. The patent with publication number US 6022419 A refers to a reactor in which the volume occupied by the solid (sawdust), decreases continuously by the effect of a spring, which pushes it towards a limb.

La patente con n° de publicación WO 201 1091044 A1 describe un procedimiento para extraer celulosa y hemicelulosa de la biomasa, con agua subcrítica y supercrítica, a través de un reactor continuo alimentado con una suspensión de agua y biomasa. La patente con n° de publicación US 6228177 B1 describe un sistema en serie, para la extracción de material lignocelulósico, en el que los reactores se enfrían mediante inmersión en agua fría. Patent No. Publication WO 201 1091044 A1 describes a process for extracting cellulose and hemicellulose from biomass, with subcritical and supercritical water, through a continuous reactor fed with a suspension of water and biomass. The patent with publication number US 6228177 B1 describes a series system, for the extraction of lignocellulosic material, in which the reactors are cooled by immersion in cold water.

También es conocida la publicación de King SD referida a "The future of industrial biorefineries". In: Forum WE, editor; 2010. Also known is the King SD publication referring to "The future of industrial biorefineries". In: Forum WE, editor; 2010

Descripción de la invención Description of the invention

Con el fin de alcanzar los objetivos y evitar los inconvenientes mencionados en los apartados anteriores la invención propone una planta piloto multilecho para fraccionamiento de biomasa que tiene por objeto extraer y fraccionar en continuo bioproductos como polifenoles, betaglucanos, cafeína y biopolímeros como la hemicelulosa, desde biomasas lignocelulósica residual y no residual de diferentes procedencias. In order to achieve the objectives and avoid the drawbacks mentioned in the preceding sections, the invention proposes a multi-pilot pilot plant for biomass fractionation which aims to continuously extract and fractionate bioproducts such as polyphenols, betaglucans, caffeine and biopolymers such as hemicellulose, from residual and non-residual lignocellulosic biomass from different sources.

Las biomasas vegetales contienen muchos productos interesantes. Algunos de estos, como los polifenoles contenidos en las semillas y hollejos de uvas, los beta-glucanos contenidos en la avena, en la cebada y en las setas, y especialmente la hemicelulosa, componente esencial de las plantas, y que figuran en todos los productos de origen vegetal, se pueden extraer sólo con agua con diferentes temperaturas. Los primeros dos compuestos mencionados tienen gran importancia en la salud y el bienestar humano: los polifenoles son compuestos con capacidad antioxidante que han despertado un gran interés en la salud y en la prevención de enfermedades asociadas a un aumento de los procesos de oxidación celular (cáncer, enfermedades cardiovasculares y enfermedades neurodegenerativas); los betaglucanos mejoran el control de la glucosa en sangre, así como los niveles de lípidos tales como el colesterol o triglicéridos. Vegetable biomass contains many interesting products. Some of these, such as the polyphenols contained in the seeds and skins of grapes, the beta-glucans contained in oats, barley and mushrooms, and especially hemicellulose, an essential component of plants, and that appear in all products of plant origin, can be extracted only with water with different temperatures. The first two compounds mentioned are of great importance in human health and well-being: polyphenols are compounds with antioxidant capacity that have aroused great interest in health and in the prevention of diseases associated with an increase in cellular oxidation processes (cancer , cardiovascular diseases and neurodegenerative diseases); betaglucans improve blood glucose control, as well as lipid levels such as cholesterol or triglycerides.

La hemicelulosa, cuando se aisla a partir de biomasa en masas moleculares por encima de los 3-5 kDa, tiene propiedades únicas. Se puede utilizar para producir películas para el envasado de aplicaciones en sustitución a los plásticos sintéticos, funciona como barreras contra la penetración de oxígeno; otra aplicación importante es la producción de aerogeles para aislar productos alimentarios. Hemicellulose, when isolated from biomass in molecular masses above 3-5 kDa, has unique properties. It can be used to produce films for packaging applications instead of synthetic plastics, it works as barriers against oxygen penetration; Another important application is the production of aerogels to isolate food products.

La xilosa a partir de la hemicelulosa, por ejemplo, se puede convertir en furfural, que es un precursor utilizado en diferentes campos, tales como el refino de petróleo, plásticos, farmacéutica y agroquímica. La xilosa puede ser también hidrogenada o enzimáticamente transformada en xilitol, que es un agente edulcorante y también se utiliza para la prevención de las caries dental. Xylose from hemicellulose, for example, can be converted into furfural, which is a precursor used in different fields, such as petroleum refining, plastics, pharmaceuticals and agrochemicals. Xylose can also be hydrogenated or enzymatically transformed into xylitol, which is a sweetening agent and is also used for the prevention of tooth decay.

La idea de la transformación de biomasa en energía, materiales y productos químicos, define el concepto de biorrefinería, tema particularmente interesante hoy en día, teniendo en cuenta las cuestiones relacionadas con los combustibles fósiles y derivados. The idea of the transformation of biomass into energy, materials and chemical products defines the concept of biorefinery, a particularly interesting topic today, taking into account issues related to fossil fuels and derivatives.

Dos categorías de materia prima dominan la investigación: primera y segunda generación. Productos de primera generación se fabrican a partir de biomasa comestible tales como plantas ricas en almidón o aceitosas; productos de segunda generación utilizan biomasa que consiste en las partes no comestibles residuales de los actuales cultivos u otras fuentes no alimentarias, como las hierbas perennes o algas. Estos son ampliamente reconocidos como poseedores de un potencial significativamente mayor para reemplazar productos de origen fósil (King, 2010). Two categories of raw material dominate research: first and second generation. First generation products are manufactured from edible biomass such as starch-rich or oily plants; second generation products use biomass that It consists of the residual inedible parts of current crops or other non-food sources, such as perennial herbs or algae. These are widely recognized as having significantly greater potential to replace fossil products (King, 2010).

Los materiales lignocelulósicos pertenecen a las materias primas de segunda generación, y se pueden obtener de varias fuentes, tales como residuos de madera, residuos agrícolas o municipales, que no interfieren con los cultivos para el consumo humano directo. Se componen principalmente de lignina, celulosa y hemicelulosa, asociadas en una estructura resistente, cuya ruptura requiere una cantidad considerable de energía; Sin embargo, gracias a su composición diferenciada, permiten obtener combustibles y múltiples productos químicos de alto valor. Lignocellulosic materials belong to second-generation raw materials, and can be obtained from various sources, such as wood waste, agricultural or municipal waste, which do not interfere with crops for direct human consumption. They consist mainly of lignin, cellulose and hemicellulose, associated in a resistant structure, whose rupture requires a considerable amount of energy; However, thanks to their differentiated composition, they allow to obtain fuels and multiple high-value chemicals.

La biomasa lignocelulósica se puede fraccionar en celulosa, hemicelulosa y lignina, a partir de las cuales se pueden producir azúcares, combustibles, materiales y productos químicos. Desde los residuos de elaboración se puede producir energía. La planta de la invención ofrece grandes mejoras en la extracción de hemicelulosa, una parte integral del proceso de biorrefinería. Además la planta de la invención incluye numerosas innovaciones para la extracción de bioproductos a partir de biomasa, y permite: Lignocellulosic biomass can be divided into cellulose, hemicellulose and lignin, from which sugars, fuels, materials and chemicals can be produced. Energy can be produced from processing waste. The plant of the invention offers great improvements in the extraction of hemicellulose, an integral part of the biorefinery process. In addition, the plant of the invention includes numerous innovations for the extraction of bioproducts from biomass, and allows:

- Extracción continua de biopolímeros y biocompuestos a partir de biomasa, con agua subcrítica (hasta 16 bar y 200 °C).  - Continuous extraction of biopolymers and biocomposites from biomass, with subcritical water (up to 16 bar and 200 ° C).

- Intercambio rápido del sólido exhausto sin parar el proceso.  - Fast exchange of the exhausted solid without stopping the process.

- Ahorro energético entre el 85% y el 95% mediante un sistema de intercambio de calor con aprovechamiento en producto y en las tomas de muestra. - Energy savings between 85% and 95% through a heat exchange system with use in the product and in the sampling.

- Posibilidad de operar con diferentes tipos de biomasa, y sin limitaciones debidas al tamaño de partículas.  - Possibility of operating with different types of biomass, and without limitations due to particle size.

- Facilidad y velocidad en la operación, contacto físico mínimo con el aparato.  - Ease and speed in operation, minimal physical contact with the device.

La planta piloto multilecho es aplicable a las industrias de procesado de café soluble; sin embargo en dichas industrias se utiliza simplemente el extractor vacío, ya que unas estructuras tubulares que incluyen dichas industrias son suficientemente grandes como para desalojar el sólido exhausto. En cambio, a nivel de planta piloto el material sólido se atasca y crea graves problemas para hacer posible una operación de extracción en continuo. Con la planta de la invención se logra cargar la biomasa en unos cartuchos que se insertan en caliente en cada reactor, de forma que una serie de válvulas logran aislar los lechos de modo que se pueda intercambiar la biomasa exhausta sin parar el proceso de fraccionamiento y extracción conseguido en la planta de la invención. The multi-strand pilot plant is applicable to the soluble coffee processing industries; however, in these industries the vacuum extractor is simply used, since tubular structures that include said industries are large enough to dislodge the exhausted solid. On the other hand, at the pilot plant level the solid material gets stuck and creates serious problems to make a continuous extraction operation possible. With the The plant of the invention is able to load the biomass into cartridges that are inserted hot in each reactor, so that a series of valves manage to isolate the beds so that the exhausted biomass can be exchanged without stopping the fractionation and extraction process achieved in the plant of the invention.

La planta piloto multilecho de la invención comprende unos reactores intercomunicados entre sí mediante un circuito de tuberías por donde fluye un fluido líquido impulsado por al menos una moto-bomba; donde los reactores incluyen unos cartuchos contenedores de la biomasa, una entrada de fluido líquido que recorre la biomasa contenida dentro de los cartuchos y una salida de fluido líquido que contiene diversas sustancias extraídas de la biomasa alojada dentro de los cartuchos. The multi-strand pilot plant of the invention comprises reactors interconnected with each other by a pipe circuit through which a liquid fluid flows driven by at least one motorcycle pump; where the reactors include biomass container cartridges, a liquid fluid inlet that runs through the biomass contained within the cartridges and a liquid fluid outlet that contains various substances extracted from the biomass housed inside the cartridges.

La planta piloto de la invención comprende además unos reactores en disposición vertical que tienen la entrada de fluido líquido por encima del cartucho, y la salida de fluido líquido está situada en una parte inferior de los reactores. The pilot plant of the invention further comprises reactors in vertical arrangement that have the liquid fluid inlet above the cartridge, and the liquid fluid outlet is located in a lower part of the reactors.

En los extremos inferiores de los reactores conectan unos dispositivos de apertura y cierre de dichos reactores ubicados por debajo de los cartuchos; donde los cartuchos se introducen dentro de los reactores y se extraen del interior de dichos reactores a través de los dispositivos de apertura y cierre cuando se sitúan en una posición abierta. At the lower ends of the reactors connect opening and closing devices of said reactors located below the cartridges; where the cartridges are introduced into the reactors and are removed from the interior of said reactors through the opening and closing devices when they are placed in an open position.

El circuito de tuberías comprende unas partes de ida por las que discurre el fluido líquido dirigido hacia las entradas de fluido líquido dentro de los reactores, y unas partes de retorno por las que discurre el fluido liquido cuando sale de los reactores; donde en dichas partes del circuito de tuberías se intercalan unas válvulas que permiten aislar de forma independiente los reactores para el intercambio de cartuchos sin detener el funcionamiento de la planta piloto. The piping circuit comprises a part of the flow through which the liquid fluid directed towards the liquid fluid inlets flows into the reactors, and some return parts through which the liquid fluid flows when it leaves the reactors; where in said parts of the piping circuit, valves are inserted that allow the isolation of the reactors for the exchange of cartridges without stopping the operation of the pilot plant.

Cada una de las partes de ida del circuito de tuberías incluye una primera válvula de tres vías y una segunda válvula de dos vías intercalada en una derivación que arranca de la entrada al reactor. Each of the outlets of the pipeline circuit includes a first three-way valve and a second two-way valve interspersed in a branch that starts from the inlet to the reactor.

Cada una de las partes de retorno del circuito de tuberías incluye al menos una primera válvula de dos vías. Una salida de la primera válvula de tres vías conecta con un tramo de tubería que alimenta al reactor; mientras que otra salida de la primera válvula de tres vías alimenta a un tramo intermedio que conecta con otra primera válvula de tres vías intercalada en otra parte de ida del circuito de tuberías. Each of the return parts of the pipeline circuit includes at least a first two-way valve. An outlet of the first three-way valve connects to a section of pipe that feeds the reactor; while another outlet of the first three-way valve feeds an intermediate section that connects with another first three-way valve interspersed in another one-way part of the pipeline circuit.

La primera válvula de dos vías está intercalada en un tramo de tubería que arranca de la salida del reactor y conecta con dicho tramo intermedio. The first two-way valve is interspersed in a pipe section that starts from the reactor outlet and connects to said intermediate section.

La planta de la invención incluye una válvula de aguja de dos posiciones intercalada en un tramo extremo de tubería que conecta con el tramo de tubería de la salida del reactor y con un intercambiador de calor que conecta con una segunda válvula de tres vías que tiene una salida que conecta con un primer tubo para tomar muestras del fluido líquido, y una segunda salida que conecta con un segundo tubo. Un tramo inicial del circuito de tuberías incluye unos intercambiadores de calor iniciales en combinación con un calentador principal ubicado a continuación de dichos intercambiadores de calor iniciales. The plant of the invention includes a two-position needle valve interspersed in an end section of pipe that connects to the pipe section of the reactor outlet and with a heat exchanger that connects to a second three-way valve that has a outlet that connects with a first tube to take samples of the liquid fluid, and a second outlet that connects with a second tube. An initial section of the pipe circuit includes initial heat exchangers in combination with a main heater located after said initial heat exchangers.

La planta piloto multilecho comprende una válvula de contrapresión para regular la presión dentro de los reactores; donde dicha válvula de contrapresión está ubicada en una derivación inicial de la parte de ida del circuito de tuberías. The multileight pilot plant comprises a back pressure valve to regulate the pressure inside the reactors; wherein said backpressure valve is located in an initial branch of the first part of the pipeline circuit.

La parte de retorno de un último reactor correspondiente con la salida de fluido líquido de dicho último reactor, conecta con una derivación de retroalimentación que desemboca en una zona inicial de la parte de ida del circuito de tuberías. The return part of a last reactor corresponding to the liquid fluid outlet of said last reactor, connects with a feedback bypass leading to an initial area of the first part of the pipe circuit.

Cada uno de los reactores tiene una salida adicional superior donde conecta una derivación de tubería que desemboca en un contenedor; donde en dicha derivación de tubería está intercalada una tercera válvula de dos vías. Each of the reactors has an additional upper outlet where it connects a pipe bypass that flows into a container; where in said pipe bypass a third two-way valve is inserted.

En una realización, cada uno de los dispositivos de apertura y cierre de los reactores comprende una válvula de esfera. In one embodiment, each of the reactors opening and closing devices comprises a ball valve.

La planta piloto comprende unos dispositivos de paracaídas fijados a los dispositivos de apertura y cierre ubicados en los extremos inferiores de los reactores; donde dichos dispositivos de paracaíadas amortiguan la caída de los cartuchos cuando se extraen del interior de los reactores. The pilot plant comprises parachute devices fixed to the opening and closing devices located at the lower ends of the reactors; where sayings Parachute devices dampen the fall of the cartridges when removed from inside the reactors.

Los reactores están revestidos homogéneamente mediante unas resistencias envolventes para calentar dichos reactores y mantener la temperatura. The reactors are homogeneously coated by wrapping resistors to heat said reactors and maintain the temperature.

Cada uno de los reactores de la planta comprende: Each of the reactors of the plant comprises:

- una malla tubular que se llena con biomasa.  - a tubular mesh that is filled with biomass.

- un carcasa tubular interior que tiene una base inferior perforada y una base superior abierta; donde dentro de dicha carcasa tubular interior se ubica la malla tubular.  - an inner tubular housing having a perforated lower base and an open upper base; where the tubular mesh is located within said inner tubular housing.

- una carcasa tubular exterior donde se aloja el cartucho constituido por la carcasa tubular interior y la malla tubular.  - an outer tubular housing where the cartridge constituted by the inner tubular housing and the tubular mesh is housed.

La malla tubular comprende dos medias partes desmontables que se acoplan entre sí a través de dos generatrices opuestas que siguen una trayectoria quebrada. The tubular mesh comprises two removable half parts that are coupled to each other through two opposite generatrices that follow a broken path.

La carcasa tubular interior comprende dos partes separadas: una primera parte que incluye la base inferior perforada, y una segunda parte que incluye un estrechamiento donde se ubica la base superior abierta. The inner tubular housing comprises two separate parts: a first part that includes the perforated lower base, and a second part that includes a narrowing where the open upper base is located.

La carcasa tubular exterior de cada reactor comprende un cuerpo principal y una tapa que cierra el cuerpo principal por su extremo superior, mientras que su extremo inferior conecta con el dispositivo de apertura y cierre; donde la tapa incluye una boca de entrada de fluido líquido dentro del reactor; y donde el cuerpo principal incluye una boca de salida de fluido líquido y la salida adicional que conecta con la derivación de tubería que desagua parte del fluido líquido en el contenedor. The outer tubular casing of each reactor comprises a main body and a cover that closes the main body at its upper end, while its lower end connects to the opening and closing device; where the cover includes a liquid fluid inlet into the reactor; and where the main body includes a liquid fluid outlet and the additional outlet that connects to the pipe bypass that drains part of the liquid fluid into the container.

En una realización de la invención, la malla tubular, carcasa tubular inferior y carcasa tubular exterior tienen una configuración cilindrica y están constituidas por un material metálico. In one embodiment of the invention, the tubular mesh, lower tubular casing and outer tubular casing have a cylindrical configuration and consist of a metallic material.

Cada intercambiador de calor ubicado en la parte de retorno del circuito de tuberías, comprende dos tubos concéntricos: exterior e interior; donde desde el tubo interior se descarga el fluido líquido contenido en el reactor, enfriado por agua que fluye por el tubo exterior. Cada uno de los dispositivos de paracaídas comprende una placa frontal que pende de al menos dos elementos de suspensión conectados a una parte del dispositivo de apertura y cierre; donde dicha placa frontal está ubicada por debajo del dispositivo de apertura y cierre para recibir el cartucho cuando se abre dicho dispositivo de apertura y cierre. Each heat exchanger located in the return part of the pipe circuit, comprises two concentric tubes: exterior and interior; where the liquid fluid contained in the reactor is cooled from the inner tube, cooled by water flowing through the outer tube. Each of the parachute devices comprises a front plate that hangs at least two suspension elements connected to a part of the opening and closing device; wherein said faceplate is located below the opening and closing device to receive the cartridge when said opening and closing device is opened.

La planta piloto comprende una primera moto-bomba que se usa al principio del proceso para llenar los reactores antes de que el circuito de tuberías se abra para llevar a cabo el proceso de extracción y fraccionamiento en continuo de los compuestos solubles de la biomasa residual y no residual. Dicha primera moto-bomba se alimenta de un fluido líquido limpio o no, contenido dentro de un primer depósito. The pilot plant comprises a first moto-pump that is used at the beginning of the process to fill the reactors before the pipeline circuit is opened to carry out the continuous extraction and fractionation process of the soluble compounds of the residual biomass and not residual Said first moto-pump is fed by a clean liquid fluid or not, contained within a first tank.

La planta piloto comprende además una segunda moto-bomba que impulsa el fluido líquido a través del circuito de tuberías para llevar a cabo el proceso de extracción y fraccionamiento en continuo de los compuestos solubles de la biomasa residual y no residual. Dicha segunda moto-bomba se alimenta de un fluido líquido contenido dentro de un segundo depósito. The pilot plant also comprises a second motorcycle pump that drives the liquid fluid through the pipeline circuit to carry out the continuous extraction and fractionation process of the soluble compounds of the residual and non-residual biomass. Said second motor-pump is fed by a liquid fluid contained within a second reservoir.

El proceso para el fraccionamiento de biomasa llevado a cabo por la planta piloto multilecho descrita comprende las siguientes fases: The process for the fractionation of biomass carried out by the multileight pilot plant described comprises the following phases:

- calentar el fluido líquido mediante los intercambiadores de calor iniciales. - heat the liquid fluid through the initial heat exchangers.

- calentar el fluido líquido mediante el calentador principal.  - heat the liquid fluid through the main heater.

- introducir el fluido líquido dentro de los reactores por encima de los cartuchos;  - introduce the liquid fluid into the reactors above the cartridges;

- calentar los reactores mediante las resistencias envolventes ubicadas alrededor de los reactores.  - heat the reactors by means of the wrapping resistors located around the reactors.

- extraer el fluido líquido del interior de los reactores. - remove the liquid fluid from inside the reactors.

- variar la temperatura del fluido extraído de los reactores a través de los intercambiadores de calor.  - vary the temperature of the fluid extracted from the reactors through the heat exchangers.

- cambiar los cartuchos de los reactores por otros nuevos sin detener el proceso.  - replace the reactor cartridges with new ones without stopping the process.

- tomar muestras del fluido extraído del interior de los reactores después de pasar por los intercambiadores de calor a través de los primeros tubos.  - take samples of the fluid extracted from the inside of the reactors after passing through the heat exchangers through the first tubes.

- recoger el fluido extraído del interior de los reactores después de pasar por los intercambiadores de calor, a través de los segundos tubos.  - collect the fluid extracted from the inside of the reactors after passing through the heat exchangers, through the second tubes.

- regular la presión dentro de los reactores 1 mediante la válvula de contrapresión.  - regulate the pressure inside the reactors 1 by means of the back pressure valve.

- canalizar parte del fluido líquido que se introduce dentro de los reactores hasta los contenedores; donde cuando se llenan dichos contendores se interrumpe el flujo de líquido hacia los contenedores. - channel part of the liquid fluid that is introduced into the reactors to the containers; where when said containers are filled the flow of liquid to the containers.

En una realización el proceso comprende una fase adicional en la que se retorna el fluido líquido extraído del último reactor hacia la parte inicial del circuito de tuberías. In one embodiment the process comprises an additional phase in which the liquid fluid extracted from the last reactor is returned to the initial part of the pipeline circuit.

A continuación para facilitar una mejor comprensión de esta memoria descriptiva y formando parte integrante de la misma, se acompaña una serie de figuras en las que con carácter ilustrativo y no limitativo se ha representado el objeto de la invención. Breve descripción de las figuras Next, in order to facilitate a better understanding of this descriptive report and forming an integral part thereof, a series of figures are attached in which the object of the invention has been represented by way of illustration and not limitation. Brief description of the figures

Figura 1.- Muestra una vista de la planta piloto multilecho para fraccionamiento de biomasa, objeto de la invención. Comprende un conjunto de reactores en combinación con otros elementos para llevar a cabo la extracción y el fraccionamiento en continuo de compuestos solubles. También es objeto de la invención el proceso para llevar a cabo el fraccionamiento de la biomasa.  Figure 1.- Shows a view of the multileight pilot plant for biomass fractionation, object of the invention. It comprises a set of reactors in combination with other elements to carry out the extraction and continuous fractionation of soluble compounds. The process for carrying out the fractionation of biomass is also an object of the invention.

Figura 2.- Muestra una vista de una parte de la planta de la invención.  Figure 2.- Shows a view of a part of the plant of the invention.

Figura 3.- Muestra una vista en explosión de uno de los reactores junto con una válvula de esfera, que forma parte de la planta de la invención.  Figure 3.- Shows an exploded view of one of the reactors together with a ball valve, which is part of the plant of the invention.

Figura 4.- Muestra una vista en sección del reactor.  Figure 4.- Shows a sectional view of the reactor.

Figura 5.- Muestra una vista en planta de una de las piezas del reactor. Figure 5.- Shows a plan view of one of the reactor parts.

Descripción de un ejemplo de realización de la invención Description of an embodiment of the invention

Considerando la numeración adoptada en las figuras, la planta piloto multilecho para fraccionamiento de biomasa comprende varios reactores 1 en disposición vertical intercomunicados entre sí mediante unas partes de ida por las que discurre un fluido líquido dirigido hacia unas entradas de fluido líquido de los reactores 1 , y unas partes de retorno por las que discurre el fluido liquido cuando sale de los reactores 1 ; donde cada uno de los reactores trabaja en serie con los demás, con la posibilidad de poder ser excluido un reactor 1 de los demás; y donde dichas partes de ida y de retorno forman parte de un circuito de tuberías por el que fluye el fluido líquido.  Considering the numbering adopted in the figures, the multileight pilot plant for biomass fractionation comprises several reactors 1 in vertical arrangement interconnected with each other by means of one-way parts through which a liquid fluid runs towards some liquid fluid inlets of the reactors 1, and return parts through which the liquid fluid flows when it leaves the reactors 1; where each of the reactors works in series with the others, with the possibility of being able to exclude one reactor 1 from the others; and where said return and return parts are part of a pipe circuit through which liquid fluid flows.

Cada uno de los reactores 1 comprende: Each of the reactors 1 comprises:

- una malla tubular 2 de metal formada por dos medias partes 2a, 2b desmontables que se acoplan entre sí a través de dos generatrices opuestas que siguen una trayectoria quebrada; donde dicha malla tubular 2 se llena con biomasa.  - a tubular metal mesh 2 formed by two removable half parts 2a, 2b that are coupled to each other through two opposite generatrices that follow a broken path; where said tubular mesh 2 is filled with biomass.

- una carcasa tubular interior 3 de acero inoxidable con una base inferior perforada 4 y una base superior abierta 5; donde dentro de dicha carcasa tubular interior 3 se ubica la malla tubular 2; y donde dicha carcasa tubular interior 3 comprende dos partes separadas: una primera parte 3a que incluye la base inferior perforada 4 y una segunda parte 3b que incluye un estrechamiento 6 donde se ubica la base superior abierta 5. - an inner tubular housing 3 made of stainless steel with a perforated bottom base 4 and a upper base open 5; wherein within said inner tubular housing 3 the tubular mesh 2 is located; and wherein said inner tubular housing 3 comprises two separate parts: a first part 3a that includes the perforated lower base 4 and a second part 3b that includes a narrowing 6 where the open upper base 5 is located.

- una carcasa tubular exterior 7 de acero inoxidable, donde se aloja el cartucho constituido por la carcasa tubular interior 3 y la malla tubular 2. Dicha carcasa tubular exterior 7 comprende un cuerpo principal 7a y una tapa 7b que cierre el cuerpo principal 7a por su extremo superior, mientras que su extremo inferior conecta con una válvula de esfera 9. En la realización que se muestra en las figuras, la malla tubular 2, carcasa tubular inferior 3 y carcasa tubular exterior 7 tienen una configuración cilindrica. - an outer tubular casing 7 of stainless steel, where the cartridge constituted by the inner tubular casing 3 and the tubular mesh 2 is housed. Said outer tubular casing 7 comprises a main body 7a and a cover 7b which closes the main body 7a by its upper end, while its lower end connects with a ball valve 9. In the embodiment shown in the figures, the tubular mesh 2, lower tubular housing 3 and outer tubular housing 7 have a cylindrical configuration.

Con esta disposición descrita, el conjunto del cartucho se inserta desde abajo dentro de la carcasa tubular exterior 7 a través de la válvula de esfera 9 cuando está en posición abierta hasta que se introduce completamente dentro de dicha carcasa tubular exterior 7. With this arrangement described, the cartridge assembly is inserted from below into the outer tubular casing 7 through the ball valve 9 when it is in the open position until it is fully inserted into said outer tubular casing 7.

En este momento la válvula de esfera 9 se cierra y al terminar la extracción haciendo pasar un fluido líquido por el interior del reactor 1 , se procede a la apertura de la válvula de esfera 9 cayendo hacia abajo por gravedad el cartucho que se extrae hacia afuera, de manera que la salida del cartucho se amortigua mediante un dispositivo de paracaídas 10 ubicado en la zona de salida de la válvula de esfera 9. At this time the ball valve 9 closes and when the extraction is finished by passing a liquid fluid through the interior of the reactor 1, the ball valve 9 is opened by dropping down the gravity of the cartridge that is drawn outwards. , so that the outlet of the cartridge is damped by a parachute device 10 located in the outlet area of the ball valve 9.

Un flujo constante de agua (u otro fluido líquido adecuado) entra por una boca de entrada 1 1 ubicada en la parte superior de cada reactor 1 realizando un recorrido hacia abajo por el interior de dicho reactor 1 hasta que sale por una boca de salida 12 situada en la parte inferior del reactor 1 ; donde la boca de entrada 11 está situada en la tapa 7b de la carcasa tubular exterior 7 y la boca de salida 12 está situada en una parte inferior del cuerpo principal 7a de dicha carcasa tubular exterior 7. El flujo líquido de salida puede ir al siguiente reactor 1 , o puede ser desviado con el fin de excluir el siguiente reactor 1 , y pasar al próximo reactor 1. De esta manera la biomasa puede ser descargada (a través de la apertura de la válvula de esfera 9 y la remoción rápida del cartucho) del reactor 1 en el que se completa el proceso de extracción, y otro reactor 1 se puede cargar con otro cartucho, luego desviar en ese reactor 1 el flujo líquido para continuar con el proceso de extracción. La planta de la invención permite un funcionamiento rápido y continuo sin paradas. A constant flow of water (or other suitable liquid fluid) enters through an inlet opening 1 1 located at the top of each reactor 1 making a downward path through the interior of said reactor 1 until it exits through an outlet port 12 located at the bottom of the reactor 1; where the inlet 11 is located in the cover 7b of the outer tubular casing 7 and the outlet 12 is located in a lower part of the main body 7a of said outer tubular casing 7. The liquid outflow can go to the next reactor 1, or it can be diverted in order to exclude the next reactor 1, and move on to the next reactor 1. In this way the biomass can be discharged (through the opening of the ball valve 9 and the rapid removal of the cartridge ) of the reactor 1 in which the extraction process is completed, and another reactor 1 can be loaded with another cartridge, then divert in that reactor 1 the liquid flow to continue with the extraction process. The plant of the invention allows operation Fast and continuous without stops.

Otra característica importante de la planta de la invención, es el ajuste de la temperatura del agua y el control de energía. Para ello, antes de entrar en los reactores 1 , el agua pasa a través de un calentador principal 13 formado por un serpentín en espiral enrollado alrededor de un cuerpo macizo metálico; donde dicho serpentín en espiral está cubierto por una resistencia eléctrica de abrazadera. Another important feature of the plant of the invention is the adjustment of water temperature and energy control. To do this, before entering the reactors 1, the water passes through a main heater 13 formed by a spiral coil wound around a solid metal body; where said spiral coil is covered by an electric clamp resistor.

El agua entra a continuación en los reactores 1 , que están revestidos homogéneamente con unas resistencias envolventes 14 de abrazadera. Después de dejar el reactor 1 , el fluido líquido entra en un intercambiador de calor 15 de tubos concéntricos. En la parte exterior fluye el suministro de agua de la planta, que se calienta previamente a través de unos intercambiadores de calor iniciales 16 y luego pasa al calentador principal 13 descrito anteriormente. Todo el sistema está aislado térmicamente con una capa de lana de vidrio cubierta con papel de aluminio. El ahorro total de calor es del 85% y el ahorro de enfriamiento está cercano al 100%. The water then enters the reactors 1, which are homogeneously coated with clamp wraps 14. After leaving the reactor 1, the liquid fluid enters a heat exchanger 15 of concentric tubes. On the outside, the water supply of the plant flows, which is previously heated through initial heat exchangers 16 and then passes to the main heater 13 described above. The entire system is thermally insulated with a layer of glass wool covered with aluminum foil. The total heat savings is 85% and the cooling savings are close to 100%.

Cada reactor 1 puede ser vaciado del fluido líquido caliente presurizado antes de extraer el cartucho constituido por la malla tubular 2 y carcasa tubular interior 3. Entre cada par de reactores 1 adyacentes se sitúa el intercambiador de calor 15 con tubos concéntricos: exterior e interior; donde desde el tubo interior se descarga el líquido contenido en el reactor 1 , enfriado por agua que fluye por el tubo exterior. Estos intercambiadores de calor 15 también permiten la toma de muestras de líquido de cada reactor durante la reacción del fluido líquido con la biomasa. Each reactor 1 can be emptied of the pressurized hot liquid fluid before removing the cartridge constituted by the tubular mesh 2 and inner tubular casing 3. Between each pair of adjacent reactors 1 is located the heat exchanger 15 with concentric tubes: outer and inner; where the liquid contained in the reactor 1, cooled by water flowing through the outer tube, is discharged from the inner tube. These heat exchangers 15 also allow the sampling of liquid from each reactor during the reaction of the liquid fluid with the biomass.

Dependiendo del compuesto que se desea extraer de los reactores, diferentes temperaturas son necesarias. Depending on the compound to be extracted from the reactors, different temperatures are necessary.

La extracción de los polifenoles requiere una temperatura entre 60 y 80 °C; la extracción de beta-glucanos alrededor de los 100 °C; mientras que la extracción de la hemicelulosa requiere temperaturas entre 1 10 y 210 °C. Por tanto, es necesario un control de la temperatura eficaz, que se realiza por medio de unos dispositivos controladores PID. The extraction of polyphenols requires a temperature between 60 and 80 ° C; the extraction of beta-glucans around 100 ° C; while hemicellulose extraction requires temperatures between 10 and 210 ° C. Therefore, an effective temperature control is necessary, which is carried out by means of PID controller devices.

Para alcanzar temperaturas por encima de 100 °C, es necesario aumentar también la presión dentro de los reactores 1 , que se regula a través de una válvula de contrapresión 17 ubicada en una derivación inicial 18 del circuito de tuberías de la planta. To reach temperatures above 100 ° C, it is also necessary to increase the pressure inside reactors 1, which is regulated through a back pressure valve 17 located in an initial branch 18 of the plant's pipeline circuit.

La planta incluye además válvulas de seguridad en cada reactor 1 que evitan cualquier sobrepresión. También se incluye un termostato que evita el sobrecalentamiento del cuerpo macizo metálico del calentador principal 13. The plant also includes safety valves in each reactor 1 that avoid any overpressure. Also included is a thermostat that prevents overheating of the solid metal body of the main heater 13.

Para que la operación de extracción sea continúa, es necesario descargar rápidamente los reactores 1. Dado que el sistema de la planta de la invención está bajo presión, una apertura repentina de la válvula de esfera 9 podría causar una fuga de vapor de agua sobrecalentado. Por esta razón, entre un reactor y otro adyacente se ha colocado el correspondiente intercambiador de calor 15 con los tubos concéntricos: exterior e interior. In order for the extraction operation to continue, it is necessary to quickly discharge the reactors 1. Since the system of the plant of the invention is under pressure, a sudden opening of the ball valve 9 could cause an overheated steam leakage. For this reason, a corresponding heat exchanger 15 with the concentric tubes has been placed between an reactor and an adjacent one: outer and inner.

Según se ha descrito anteriormente, desde el tubo interior se descarga el líquido contenido en el reactor 1 después de la operación de extracción, y por el tubo exterior fluye agua fría que luego alimenta a la planta de la invención. As described above, the liquid contained in the reactor 1 is discharged from the inner tube after the extraction operation, and cold water flows through the outer tube which then feeds the plant of the invention.

Al principio del proceso, la biomasa se introduce dentro de la malla tubular 2, que se puede abrir longitudinalmente, y que se inserta entre las dos partes 3a, 3b de la carcasa tubular interior 3. La primera parte 3a está abierta por el extremo superior y por el extremo inferior tiene la base inferior perforada 4 con orificios de diámetro entre 5 mm y 0.5 mm. Según se ha referido anteriormente, el conjunto de la malla tubular 2 y de la carcasa tubular interior 3 se inserta, a través de la válvula de esfera 9, dentro de la carcasa tubular exterior 7 cerrada por la extremidad superior mediante la tapa 8 que se puede remover en el caso de que se atasque el reactor 1. At the beginning of the process, the biomass is introduced into the tubular mesh 2, which can be opened longitudinally, and inserted between the two parts 3a, 3b of the inner tubular casing 3. The first part 3a is open at the upper end and at the lower end it has the perforated lower base 4 with holes with a diameter between 5 mm and 0.5 mm. As mentioned above, the assembly of the tubular mesh 2 and the inner tubular casing 3 is inserted, through the ball valve 9, into the outer tubular casing 7 closed by the upper end by the cover 8 which is It can be removed if reactor 1 becomes clogged.

El tamaño de las partículas de biomasa cargadas en el reactor 1 , tiene que ser superior al tamaño del diámetro de los orificios de la base inferior perforada 4 de la carcasa tubular interior 3, que funciona como un filtro impidiendo que la biomasa solida sea removida del lecho y arrastrada a través de los distintos elementos de la planta de la invención. The size of the biomass particles loaded in the reactor 1 has to be larger than the diameter of the holes of the perforated bottom base 4 of the inner tubular casing 3, which functions as a filter preventing solid biomass from being removed from the bed and dragged through the different elements of the plant of the invention.

En una realización como la mostrada en las figuras 2 y 3, la planta de la invención comprende una unidad operativa de reactor 1 donde se lleva a cabo el proceso para el fraccionamiento de la biomasa. In an embodiment such as that shown in Figures 2 and 3, the plant of the invention comprises an operating unit of reactor 1 where the process for biomass fractionation is carried out.

En cambio, en la figura 1 , se muestra una planta que incluye varias unidades de reactores conectados, que pueden operar en serie uno con otro, o por separado, y donde también se lleva a cabo el proceso para el fraccionamiento de la biomasa. On the other hand, in figure 1, a plant is shown that includes several connected reactor units, which can operate in series with one another, or separately, and where also carries out the process for the fractionation of biomass.

Una vez que un reactor 1 se ha cargado con la biomasa, como se ha descrito anteriormente, se empuja el cartucho hasta que entra completamente, y posteriormente se cierra la válvula de esfera 9 situada por debajo del cartucho. En este momento, se llena el reactor 1 con agua, impulsada mediante una primera moto-bomba 19, asegurándose de que el líquido entra en el reactor 1 y no se escapa a través del circuito de tuberías. Once a reactor 1 has been loaded with the biomass, as described above, the cartridge is pushed until it enters completely, and then the ball valve 9 located below the cartridge is closed. At this time, the reactor 1 is filled with water, driven by a first motor pump 19, making sure that the liquid enters the reactor 1 and does not leak through the pipeline circuit.

Por esta razón, se aisla cada reactor 1 del resto del sistema de la planta piloto mediante el cierre de una primera válvula 20 de dos vías y una segunda válvula de aguja 21 situadas a la salida de cada reactor 1. También se abre una segunda válvula 22 de dos vías y se mueve una primera válvula 23 de tres vías, de manera tal que el agua entre sólo en un reactor 1 , y en el segmento de tubo entre el reactor y dicha primera válvula 23 de tres vías. La primera válvula 23 de tres vías puede desviar el flujo hacia el siguiente reactor 1 o hacia la siguiente primera válvula 23 de tres vías, evitando el reactor 1 anterior. For this reason, each reactor 1 is isolated from the rest of the pilot plant system by closing a first two-way valve 20 and a second needle valve 21 located at the exit of each reactor 1. A second valve is also opened 22 two-way and a first three-way valve 23 is moved, such that water enters only in a reactor 1, and in the tube segment between the reactor and said first three-way valve 23. The first three-way valve 23 can divert the flow to the next reactor 1 or to the next first three-way valve 23, avoiding the previous reactor 1.

Una tercera válvula 24 de dos vías conectada a una salida adicional superior 25 de cada reactor 1 , se mantiene abierta hasta que se comprueba que un contenedor 26 empieza a llenarse de fluido líquido a través de una derivación de tubería que arranca de dicha tercera válvula 24 y desemboca en el contenedor 26. En ese momento se cierran las válvulas de dos vías 22 y 24, y se desconecta la primera moto-bomba 19 interrumpiendo el flujo de fluido líquido hacia el reactor 1. En esta situación, la biomasa contenida dentro del reactor 1 está completamente sumergida en el fluido líquido, y el reactor 1 está aislado del sistema de la planta piloto. A third two-way valve 24 connected to an additional upper outlet 25 of each reactor 1, remains open until it is found that a container 26 begins to fill with liquid fluid through a pipe bypass that starts from said third valve 24 and empties into the container 26. At that time the two-way valves 22 and 24 are closed, and the first motorcycle pump 19 is disconnected interrupting the flow of liquid fluid to the reactor 1. In this situation, the biomass contained within the reactor 1 is completely submerged in the liquid fluid, and reactor 1 is isolated from the pilot plant system.

El reactor 1 se calienta homogéneamente mediante las resistencias envolventes 14 hasta una temperatura ligeramente inferior a la temperatura mínima que se necesita para empezar la extracción del compuesto que se quiere extraer. The reactor 1 is heated homogeneously by the wrapping resistors 14 to a temperature slightly below the minimum temperature needed to begin the extraction of the compound to be extracted.

La hemicelulosa empieza a extraerse a temperaturas superiores a 100 °C; de manera que si se decide extraer dicho compuesto de hemicelulosa hay que precalentar el reactor 1 y esperar a que el reactor 1 alcance temperaturas superiores a 100 °C. Una segunda moto-bomba 27 se activa para impulsar el flujo de líquido que pasa previamente a través de los intercambiadores de calor iniciales 16, funcionando como un liquido de enfriamiento de otro líquido caliente que sale del sistema, y al mismo tiempo consiguiendo un primer precalentamiento. Consecutivamente consigue un ulterior precalentamiento, mediante el calentador principal 13, hacia una temperatura superior a la cual se requiere operar; siguiendo el fluido líquido después hacia la primera válvula 23 de tres vías. Hemicellulose begins to be extracted at temperatures above 100 ° C; so that if it is decided to extract said hemicellulose compound, the reactor 1 must be preheated and wait for the reactor 1 to reach temperatures above 100 ° C. A second motorcycle pump 27 is activated to drive the flow of liquid that previously passes through the initial heat exchangers 16, functioning as a cooling liquid of another hot liquid leaving the system, and at the same time achieving a first preheating . Consequently, it achieves further preheating, by means of the main heater 13, towards a temperature higher than the one required to operate; following the liquid fluid then to the first three-way valve 23.

Como se ha referido anteriormente, en una realización, dicha primera válvula 23 de tres vías sigue colocada en una posición en la que el flujo de líquido es desviado hacia la siguiente primera válvula 23 de tres vías, y no hacia el reactor 1. As mentioned above, in one embodiment, said first three-way valve 23 is still placed in a position where the flow of liquid is diverted to the next first three-way valve 23, and not to the reactor 1.

Cuando el flujo alcanza la temperatura requerida, se sube la temperatura del reactor hacia las condiciones con las cuales se quiere operar; ajustándose la primera válvula 23 de tres vías, de manera que el flujo de líquido entre en el reactor 1 , y al mismo tiempo se abre la primera válvula 20 de dos vías para que el líquido pueda salir del reactor 1. En este momento empieza la extracción de los compuestos solubles desde la biomasa en el reactor 1 : el flujo de líquido entra en el reactor 1 , pasa a través del lecho de biomasa, extrae los compuestos solubles, y sale del reactor. When the flow reaches the required temperature, the reactor temperature is raised to the conditions under which it is desired to operate; the first three-way valve 23 being adjusted, so that the flow of liquid enters the reactor 1, and at the same time the first two-way valve 20 is opened so that the liquid can leave the reactor 1. At this time the extraction of the soluble compounds from the biomass in the reactor 1: the liquid flow enters the reactor 1, passes through the biomass bed, extracts the soluble compounds, and leaves the reactor.

El proceso descrito hasta ahora, se refiere básicamente al funcionamiento de una sola unidad de reactor 1. The process described so far basically refers to the operation of a single reactor unit 1.

El flujo de líquido que sale del reactor 1 llega a otra primera válvula 23 de tres vías, de manera que actuando sobre esta primera válvula 23 de tres vías se puede dirigir el flujo al siguiente reactor 1 o hacia la siguiente primera válvula 23 de tres vías. Esta operación se puede repetir para cada unidad de reactor en el sistema de la planta piloto. De esta manera, cada reactor 1 se puede integrar en el proceso de extracción, o se puede omitir. Después de salir del último reactor 1 utilizado en el sistema de la planta piloto, la corriente de líquido caliente es devuelta y entra en la parte interior de los intercambiadores de calor iniciales 16 transfiriendo calor al líquido alimentado en el sistema. La salida de líquido, por lo tanto se enfría, y se despresuriza a través de la válvula de contrapresión 17, y finalmente sale del sistema. La válvula de contrapresión 17 regula la presión de todo el sistema de extracción, de manera que cuando se desea interrumpir la reacción en un reactor 1 , se desvía el flujo de líquido, bloqueando el suministro a la unidad de reactor 1 correspondiente para ser aislado del sistema. The flow of liquid leaving the reactor 1 reaches another first three-way valve 23, so that by acting on this first three-way valve 23, the flow can be directed to the next reactor 1 or to the next first three-way valve 23 . This operation can be repeated for each reactor unit in the pilot plant system. In this way, each reactor 1 can be integrated into the extraction process, or it can be omitted. After leaving the last reactor 1 used in the pilot plant system, the hot liquid stream is returned and enters the inside of the initial heat exchangers 16 transferring heat to the liquid fed into the system. The liquid outlet, therefore, cools, and depressurizes through the back pressure valve 17, and finally exits the system. The back pressure valve 17 regulates the pressure of the entire extraction system, so that when it is desired to interrupt the reaction in a reactor 1, the flow of liquid is diverted, blocking the supply to the corresponding reactor unit 1 to be isolated from the system.

Para ello, se gira la primera válvula 23 de tres vías que precede al respectivo reactor 1 y se cierra la primera válvula 20 de dos vías colocada a la salida de dicho reactor 1 , excluyendo así el correspondiente reactor 1 del sistema. El flujo de líquido puede ser dirigido a la unidad de reactor 1 subsiguiente (cargado con un cartucho de biomasa, como se ha explicado anteriormente), o puede ser dirigido a la primera válvula 23 de tres vías siguiente, que a su vez puede dirigir el flujo. For this, the first three-way valve 23 that precedes the respective reactor 1 is rotated and the first two-way valve 20 placed at the exit of said reactor 1 is closed, thus excluding the corresponding reactor 1 from the system. The liquid flow can be directed to the subsequent reactor unit 1 (loaded with a biomass cartridge, as explained above), or it can be directed to the next three-way first valve 23, which in turn can direct the flow.

La válvula de aguja 21 tiene una salida que desemboca en el intercambiador de calor 15, de manera que cuando se abre dicha válvula de aguja 21 , el líquido contenido en el reactor 1 pasa al intercambiador de calor 15 y se enfría mediante otro líquido que fluye en la parte exterior del intercambiador de calor 15. De esta manera, el líquido presurizado contenido dentro del reactor no se vaporiza durante la apertura de la válvula de aguja 15, y sale como un líquido normal sin presión. The needle valve 21 has an outlet that flows into the heat exchanger 15, so that when said needle valve 21 is opened, the liquid contained in the reactor 1 passes to the heat exchanger 15 and is cooled by another flowing liquid on the outside of the heat exchanger 15. In this way, the pressurized liquid contained within the reactor does not vaporize during the opening of the needle valve 15, and exits as a normal liquid without pressure.

Este sistema de la planta piloto permite vaciar completamente cada reactor del líquido, una vez que se termina el proceso de extracción. This pilot plant system allows to completely empty each reactor of the liquid, once the extraction process is completed.

A la salida del intercambiador de calor 15 se conecta una segunda válvula 28 de tres vías que permite dirigir el líquido que sale hacia un primer tubo 29 más corto para tomar una muestra del producto, o hacia un segundo tubo 30 más largo conectado a un sistema de desagüe. At the outlet of the heat exchanger 15 a second three-way valve 28 is connected which allows the liquid to be directed to a shorter first tube 29 to take a sample of the product, or to a second longer tube 30 connected to a system Drain

Después de vaciar el reactor 1 del líquido, se abre la válvula de esfera 9 por debajo del reactor 1 , haciendo que el cartucho que contiene la biomasa exhausta, caiga en el dispositivo de paracaídas 10. En esta situación, el cartucho puede ser retirado y abierto, de manera que la mala tubular 2 se extrae del interior de la carcasa tubular interior 3 y posteriormente se abre la malla tubular 2 longitudinalmente, para que se pueda recoger toda la biomasa en estado sólido. Cuando un reactor termina su funcionamiento, y se extrae el cartucho, otro cartucho contenedor de la biomasa fresca se puede volver a cargar rápidamente, reiniciando el proceso de extracción en el nuevo cartucho montado. After emptying the reactor 1 from the liquid, the ball valve 9 is opened below the reactor 1, causing the cartridge containing the exhausted biomass to fall into the parachute device 10. In this situation, the cartridge can be removed and open, so that the bad tubular 2 is removed from the inside of the inner tubular housing 3 and subsequently the tubular mesh 2 is opened longitudinally, so that all the biomass can be collected in a solid state. When a reactor finishes its operation, and the cartridge is removed, another cartridge Fresh biomass container can be quickly reloaded, restarting the extraction process in the new mounted cartridge.

La parte de retorno del último reactor 1 correspondiente con la salida de fluido líquido de dicho último reactor 1 , conecta con una derivación de retroalimentación 8 que desemboca en una zona inicial de la parte de ida del circuito de tuberías. The return part of the last reactor 1 corresponding to the liquid fluid outlet of said last reactor 1, connects with a feedback bypass 8 which flows into an initial area of the first part of the pipe circuit.

La primera moto-bomba 19 se usa al principio del proceso para llenar los reactores 1 antes de que el circuito de tuberías se abra para llevar a cabo el proceso de extracción y fraccionamiento en continuo de los compuestos solubles de la biomasa residual y no residual. Dicha primera moto-bomba 19 se alimenta de un fluido líquido limpio o no, contenido dentro de un primer depósito 31. The first motor pump 19 is used at the beginning of the process to fill the reactors 1 before the pipeline circuit is opened to carry out the process of continuous extraction and fractionation of the soluble compounds of the residual and non-residual biomass. Said first motor pump 19 is fed by a clean or not liquid fluid, contained within a first tank 31.

En cambio la segunda moto-bomba 27 impulsa el fluido líquido a través del circuito de tuberías para llevar a cabo el proceso de extracción y fraccionamiento en continuo de los compuestos solubles de la biomasa residual y no residual. Dicha segunda moto-bomba 27 se alimenta de un fluido líquido contenido dentro de un segundo depósito 32. On the other hand, the second motor pump 27 drives the liquid fluid through the piping circuit to carry out the process of continuous extraction and fractionation of the soluble compounds of the residual and non-residual biomass. Said second motor pump 27 is fed with a liquid fluid contained within a second tank 32.

Por tanto las dos moto-bombas 19, 27 se alimentan de forma independiente de fluidos líquidos contenidos dentro de los depósitos 31 , 32; que en una realización de la invención dichos fluidos líquidos son agua. Therefore, the two motor pumps 19, 27 are fed independently of liquid fluids contained within the tanks 31, 32; that in one embodiment of the invention said liquid fluids are water.

Cada uno de los dispositivos de paracaídas 10 comprende una placa frontal 10a de metal que pende de dos elementos de suspensión 10b conectados a una parte de la válvula de esfera 9; donde dicha placa frontal 10a está ubicada por debajo de dicha válvula de esfera 9. En una realización de la invención los elementos de suspensión 10b comprenden unas cadenas y en otra realización comprenden por ejemplo unos tirantes. Con esta disposición descrita, la placa frontal 10a se puede mover hacia adelante o hacia atrás para permitir la entrada y salida del cartucho. En el momento de remoción del cartucho, la placa frontal 10a se posiciona justo por debajo de la válvula de esfera 9 para recibir el cartucho que cae hacia abajo por gravedad directamente sobre dicha placa frontal 10a. Each of the parachute devices 10 comprises a metal faceplate 10a that hangs on two suspension elements 10b connected to a part of the ball valve 9; wherein said faceplate 10a is located below said ball valve 9. In one embodiment of the invention the suspension elements 10b comprise chains and in another embodiment comprise for example braces. With this arrangement described, the faceplate 10a can be moved forward or backward to allow entry and exit of the cartridge. At the time of removal of the cartridge, the faceplate 10a is positioned just below the ball valve 9 to receive the cartridge that falls down by gravity directly onto said faceplate 10a.

Claims

REIVINDICACIONES 1. - Planta piloto multilecho para fraccionamiento de biomasa, que comprende unos reactores intercomunicados entre sí mediante un circuito de tuberías por donde fluye un fluido líquido impulsado por al menos una moto-bomba; donde los reactores incluyen unos cartuchos contenedores de la biomasa, una entrada de fluido líquido que recorre la biomasa contenida dentro de los cartuchos y una salida de fluido líquido que contiene diversas sustancias extraídas de la biomasa alojada dentro de los cartuchos; caracterizada por que:1. - Multilecho pilot plant for biomass fractionation, which comprises reactors interconnected with each other by means of a pipe circuit through which a liquid fluid flows driven by at least one motorcycle pump; where the reactors include biomass container cartridges, a liquid fluid inlet that runs through the biomass contained within the cartridges and a liquid fluid outlet that contains various substances extracted from the biomass housed inside the cartridges; characterized by: - comprende unos reactores (1) en disposición vertical que tienen la entrada de fluido líquido por encima de los cartuchos, y la salida de fluido líquido está situada en una parte inferior de los reactores (1); - it comprises reactors (1) in vertical arrangement that have the liquid fluid inlet above the cartridges, and the liquid fluid outlet is located in a lower part of the reactors (1); - en los extremos inferiores de los reactores (1) conectan unos dispositivos de apertura y cierre de dichos reactores (1) ubicados por debajo de los cartuchos; donde los cartuchos se introducen dentro de los reactores (1) y se extraen del interior de dichos reactores a través de los dispositivos de apertura y cierre cuando se sitúan en una posición abierta; - at the lower ends of the reactors (1) connect opening and closing devices of said reactors (1) located below the cartridges; where the cartridges are introduced into the reactors (1) and are removed from the interior of said reactors through the opening and closing devices when they are placed in an open position; - el circuito de tuberías comprende unas partes de ida por las que discurre el fluido líquido dirigido hacia las entradas de fluido líquido dentro de los reactores (1), y unas partes de retorno por las que discurre el fluido liquido cuando sale de los reactores 1 ; donde en dichas partes del circuito de tuberías se intercalan unas válvulas que permiten aislar de forma independiente los reactores (1) para el intercambio de cartuchos sin detener el funcionamiento de la planta piloto. - the piping circuit comprises some flow parts through which the liquid fluid directed towards the liquid fluid inlets flows into the reactors (1), and return parts through which the liquid fluid flows when it leaves the reactors 1 ; where in said parts of the piping circuit, valves are inserted that allow the reactors (1) to be isolated independently for the exchange of cartridges without stopping the operation of the pilot plant. 2. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que: 2. - Multilecho pilot plant for biomass fractionation, according to claim 1, characterized in that: - cada una de las partes de ida del circuito de tuberías incluye una primera válvula (23) de tres vías y una segunda válvula (22) de dos vías intercalada en una derivación que arranca de la entrada al reactor; - each of the outlets of the pipeline circuit includes a first three-way valve (23) and a second two-way valve (22) interspersed in a branch that starts from the inlet to the reactor; - cada una de las partes de retorno del circuito de tuberías incluye al menos una primera válvula (20) de dos vías;  - each of the return parts of the pipeline circuit includes at least a first two-way valve (20); donde, where, - una salida de la primera válvula (23) de tres vías conecta con un tramo de tubería que alimenta al reactor (1); mientras que otra salida de la primera válvula (23) de tres vías alimenta a un tramo intermedio que conecta con otra primera válvula (23) de tres vías intercalada en otra parte de ida del circuito de tuberías;  - an outlet of the first three-way valve (23) connects to a section of pipe that feeds the reactor (1); while another outlet of the first three-way valve (23) feeds an intermediate section that connects with another first three-way valve (23) interspersed in another one-way part of the pipeline circuit; - la primera válvula (20) de dos vías está intercalada en un tramo de tubería que arranca de la salida del reactor (1) y conecta con dicho tramo intermedio. - the first two-way valve (20) is interspersed in a section of pipe that starts of the reactor outlet (1) and connects with said intermediate section. 3.- Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que incluye una válvula de aguja (21) de dos posiciones intercalada en un tramo extremo de tubería que conecta con el tramo de tubería de la salida del reactor (1) y con un intercambiador de calor (15) que conecta con una segunda válvula (28) de tres vías que tiene una salida que conecta con un primer tubo (29) para tomar muestras del fluido líquido, y una segunda salida que conecta con un segundo tubo (30). 3. Multi-band pilot plant for biomass fractionation, according to claim 1, characterized in that it includes a two-position needle valve (21) interspersed in an end pipe section connecting with the pipe section of the reactor outlet ( 1) and with a heat exchanger (15) that connects to a second three-way valve (28) that has an outlet that connects to a first tube (29) to sample liquid fluid, and a second outlet that connects to a second tube (30). 4.- Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 2, caracterizada por que un tramo inicial del circuito de tuberías incluye unos intercambiadores de calor iniciales (16) en combinación con un calentador principal (13) ubicado a continuación de dichos intercambiadores de calor iniciales (16). 4. Multi-band pilot plant for biomass fractionation, according to claim 2, characterized in that an initial section of the pipe circuit includes initial heat exchangers (16) in combination with a main heater (13) located next to said exchangers initial heat (16). 5.- Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que comprende una válvula de contrapresión (17) para regular la presión dentro de los reactores (1); donde dicha válvula de contrapresión (17) está ubicada en una derivación inicial (18) de la parte de ida del circuito de tuberías. 5. Multi-band pilot plant for biomass fractionation according to claim 1, characterized in that it comprises a back pressure valve (17) for regulating the pressure inside the reactors (1); wherein said back pressure valve (17) is located in an initial branch (18) of the first part of the pipeline circuit. 6.- Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que la parte de retorno de un último reactor (1) correspondiente con la salida de fluido líquido de dicho último reactor (1), conecta con una derivación de retroalimentación (8) que desemboca en una zona inicial de la parte de ida del circuito de tuberías. 6. Multi-strand pilot plant for biomass fractionation, according to claim 1, characterized in that the return part of a last reactor (1) corresponding to the liquid fluid outlet of said last reactor (1), connects with a bypass of feedback (8) leading to an initial area of the first part of the pipeline circuit. 7. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que cada uno de los reactores (1) tiene una salida adicional superior (25) donde conecta una derivación de tubería que desemboca en un contenedor (26); donde en dicha derivación de tubería está intercalada una tercera válvula (24) de dos vías. 7. - Multileight pilot plant for biomass fractionation, according to claim 1, characterized in that each of the reactors (1) has an additional upper outlet (25) where it connects a pipe branch that flows into a container (26); where in said pipe bypass a third two-way valve (24) is inserted. 8. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que cada uno de los dispositivos de apertura y cierre de los reactores (1) comprende una válvula de esfera (9). 8. - Multilecho pilot plant for biomass fractionation, according to claim 1, characterized in that each of the reactors opening and closing devices (1) comprises a ball valve (9). 9.- Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que comprende unos dispositivos de paracaídas (10) fijados a los dispositivos de apertura y cierre ubicados en los extremos inferiores de los reactores (1); donde dichos dispositivos de paracaíadas (10) amortiguan la caída de los cartuchos cuando se extraen del interior de los reactores (1). 9.- Multilecho pilot plant for biomass fractionation, according to claim 1, characterized in that it comprises parachute devices (10) fixed to the opening and closing devices located at the lower ends of the reactors (1); where said parachute devices (10) dampen the fall of the cartridges when they are removed from inside the reactors (1). 10.- Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizado por que los reactores (1) están revestidos homogéneamente mediante unas resistencias envolventes (14) para calentar dichos reactores (1) y mantener la temperatura. 10. Multi-strand pilot plant for biomass fractionation, according to claim 1, characterized in that the reactors (1) are homogeneously coated by enveloping resistors (14) to heat said reactors (1) and maintain the temperature. 11.- Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizado por que cada uno de los reactores (1) comprende: 11.- Multilecho pilot plant for biomass fractionation, according to claim 1, characterized in that each of the reactors (1) comprises: - una malla tubular (2) que se llena con biomasa;  - a tubular mesh (2) that is filled with biomass; - un carcasa tubular interior (3) que tiene una base inferior perforada (4) y una base superior abierta (5); donde dentro de dicha carcasa tubular interior (3) se ubica la malla tubular (2);  - an inner tubular housing (3) having a perforated lower base (4) and an open upper base (5); wherein within said inner tubular housing (3) the tubular mesh (2) is located; - una carcasa tubular exterior (7) donde se aloja el cartucho constituido por la carcasa tubular interior (3) y la malla tubular (2).  - an outer tubular casing (7) where the cartridge consisting of the inner tubular casing (3) and the tubular mesh (2) is housed. 12. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 1 , caracterizada por que la malla tubular (2) comprende dos medias partes (2a, 2b) desmontables que se acoplan entre sí a través de dos generatrices opuestas que siguen una trayectoria quebrada. 12. - Multileight pilot plant for biomass fractionation, according to claim 1, characterized in that the tubular mesh (2) comprises two removable half parts (2a, 2b) that are coupled to each other through two opposite generatrices that follow a broken path. 13. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 1 , caracterizada por que la carcasa tubular interior (3) comprende dos partes separadas: una primera parte (3a) que incluye la base inferior perforada (4), y una segunda parte (3b) que incluye un estrechamiento (6) donde se ubica la base superior abierta (5). 13. - Multileight pilot plant for biomass fractionation, according to claim 1, characterized in that the inner tubular housing (3) comprises two separate parts: a first part (3a) that includes the perforated lower base (4), and a second part (3b) that includes a narrowing (6) where the open upper base (5) is located. 14. - Planta piloto multilecho para fraccionamiento de biomasa, según las reivindicaciones 7 y 11 , caracterizada por que la carcasa tubular exterior (7) de cada reactor14. - Multileight pilot plant for biomass fractionation, according to claims 7 and 11, characterized in that the outer tubular casing (7) of each reactor (1) comprende un cuerpo principal (7a) y una tapa (7b) que cierra el cuerpo principal (7a) por su extremo superior, mientras que su extremo inferior conecta con el dispositivo de apertura y cierre; donde la tapa (7b) incluye una boca de entrada (11) de fluido líquido dentro del reactor (1); y donde el cuerpo principal (7a) incluye una boca de salida (12) de fluido líquido y la salida adicional (25) que conecta con la derivación de tubería que desagua parte del fluido líquido en el contenedor (26). (1) comprises a main body (7a) and a cover (7b) that closes the main body (7a) by its upper end, while its lower end connects with the opening and closing device; where the cover (7b) includes an inlet (11) of liquid fluid inside the reactor (1); and where the main body (7a) includes an outlet (12) of liquid fluid and the additional outlet (25) that connects to the pipe bypass that drains part of the liquid fluid in the container (26). 15. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 1 , caracterizada por que la malla tubular (2), carcasa tubular inferior (3) y carcasa tubular exterior (7) tienen una configuración cilindrica y están constituidas por un material metálico. 15. - Multileight pilot plant for biomass fractionation, according to claim 1, characterized in that the tubular mesh (2), lower tubular shell (3) and outer tubular shell (7) have a cylindrical configuration and consist of a material metal. 16. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 3, caracterizada por que cada intercambiador de calor (15), ubicado en la parte de retorno del circuito de tuberías, comprende dos tubos concéntricos: exterior e interior; donde desde el tubo interior se descarga el fluido líquido contenido en el reactor (1), enfriado por agua que fluye por el tubo exterior. 16. - Multileight pilot plant for biomass fractionation, according to claim 3, characterized in that each heat exchanger (15), located in the return part of the pipe circuit, comprises two concentric tubes: exterior and interior; where the liquid fluid contained in the reactor (1), cooled by water flowing through the outer tube, is discharged from the inner tube. 17. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 9, caracterizada por que cada uno de los dispositivos de paracaídas (10) comprende una placa frontal (10a) que pende de al menos dos elementos de suspensión (10b) conectados a una parte del dispositivo de apertura y cierre; donde dicha placa frontal (10a) está ubicada por debajo del dispositivo de apertura y cierre. 17. - Multileight pilot plant for biomass fractionation, according to claim 9, characterized in that each of the parachute devices (10) comprises a front plate (10a) that hangs at least two suspension elements (10b) connected to a part of the opening and closing device; wherein said front plate (10a) is located below the opening and closing device. 18. - Planta piloto multilecho para fraccionamiento de biomasa, según la reivindicación 1 , caracterizada por que comprende: 18. - Multilecho pilot plant for biomass fractionation, according to claim 1, characterized in that it comprises: - una primera moto-bomba (19) para llenar los reactores (1); donde dicha primera moto- bomba (19) se alimenta de un fluido líquido contenido dentro de un primer depósito (31); - a first motorcycle pump (19) to fill the reactors (1); wherein said first motor pump (19) feeds on a liquid fluid contained within a first reservoir (31); - una segunda moto-bomba (27) que impulsa el fluido líquido a través del circuito de tuberías; donde dicha segunda moto-bomba (27) se alimenta de un fluido líquido contenido dentro de un segundo depósito (32). - a second motorcycle pump (27) that drives the liquid fluid through the pipeline circuit; wherein said second motor pump (27) feeds on a liquid fluid contained within a second reservoir (32). 19. - Proceso para el fraccionamiento de biomasa, llevado a cabo por la planta piloto multilecho descrita en una las reivindicaciones anteriores 1 a 18, caracterizado por que comprende las fases: 19. - Process for the fractionation of biomass, carried out by the multileight pilot plant described in one of the preceding claims 1 to 18, characterized in that it comprises the phases: - calentar el fluido líquido mediante los intercambiadores de calor iniciales (16); - heating the liquid fluid by means of the initial heat exchangers (16); - calentar el fluido líquido mediante el calentador principal (13);  - heating the liquid fluid by means of the main heater (13); - introducir el fluido líquido dentro de los reactores (1) por encima de los cartuchos;  - introduce the liquid fluid into the reactors (1) above the cartridges; - calentar los reactores (1) mediante las resistencias envolventes (14) dispuestas alrededor de los reactores (1);  - heating the reactors (1) by means of the wrapping resistors (14) arranged around the reactors (1); - extraer el fluido líquido del interior de los reactores (1); - variar la temperatura del fluido extraído de los reactores (1) a través de los intercambiadores de calor (15); - extract the liquid fluid from inside the reactors (1); - varying the temperature of the fluid extracted from the reactors (1) through the heat exchangers (15); - cambiar los cartuchos de los reactores (1) por otros nuevos sin detener el proceso;  - replace the reactors cartridges (1) with new ones without stopping the process; - tomar muestras del fluido extraído del interior de los reactores después de pasar por los intercambiadores de calor (15) a través de los primeros tubos (29);  - take samples of the fluid extracted from the interior of the reactors after passing through the heat exchangers (15) through the first tubes (29); - recoger el fluido extraído del interior de los reactores (1) después de pasar por los intercambiadores de calor (15), a través de los segundos tubos (30);  - collecting the fluid extracted from inside the reactors (1) after passing through the heat exchangers (15), through the second tubes (30); - regular la presión dentro de los reactores (1) mediante la válvula de contrapresión;  - regulate the pressure inside the reactors (1) by means of the back pressure valve; - canalizar parte del fluido líquido que se introduce dentro de los reactores (1) hasta los contenedores (26); donde cuando se llenan dichos contendores (26) se interrumpe el flujo de líquido hacia los contenedores (26).  - channel part of the liquid fluid that is introduced into the reactors (1) to the containers (26); where when said containers are filled (26) the flow of liquid to the containers (26) is interrupted. 20.- Proceso para el fraccionamiento de biomasa, según la reivindicación 19, caracterizado por que comprende una fase adicional de retornar del fluido líquido extraído del último reactor (1) hacia la parte inicial del circuito de tuberías. 20. Process for the fractionation of biomass, according to claim 19, characterized in that it comprises an additional phase of returning the liquid fluid extracted from the last reactor (1) towards the initial part of the piping circuit.
PCT/ES2017/070611 2016-09-14 2017-09-14 Multi-bed pilot plant and process for biomass fractionation Ceased WO2018050941A1 (en)

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Citations (4)

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WO2011091044A1 (en) * 2010-01-19 2011-07-28 Sriya Innovations, Inc. Production of fermentable sugars and lignin from biomass using supercritical fluids
WO2012103582A1 (en) * 2011-02-01 2012-08-09 Australian Biorefining Pty Ltd Cellulose phosphate powder product and process for manufacture thereof, and application to removal of contaminants from aqueous solutions
WO2013050139A1 (en) * 2011-10-06 2013-04-11 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Adsorbent for removing fluorinated organic compounds from contaminated fluids, method of production and use thereof for removing fluorinated organic compounds from contaminated fluids

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000061276A1 (en) * 1999-04-14 2000-10-19 Midwest Research Institute Aqueous fractionation of biomass based on novel carbohydrate hydrolysis kinetics
WO2011091044A1 (en) * 2010-01-19 2011-07-28 Sriya Innovations, Inc. Production of fermentable sugars and lignin from biomass using supercritical fluids
WO2012103582A1 (en) * 2011-02-01 2012-08-09 Australian Biorefining Pty Ltd Cellulose phosphate powder product and process for manufacture thereof, and application to removal of contaminants from aqueous solutions
WO2013050139A1 (en) * 2011-10-06 2013-04-11 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Adsorbent for removing fluorinated organic compounds from contaminated fluids, method of production and use thereof for removing fluorinated organic compounds from contaminated fluids

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