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
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Prior art keywords
reactors
reactor
biomass
pilot
plant
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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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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08HDERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H8/00Macromolecular compounds derived from lignocellulosic materials

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

Multibed PROCESS AND PILOT PLANT FOR BIOMASS FRACTIONATION

DESCRIPTION OBJECT OF THE INVENTION

The present invention, as expressed in the title of this specification, relates to a process and multibed pilot for fractionating biomass, which is extracted and fractionated into soluble compounds continuous residual biomass and no residual, using as solvent water plant or water with a low concentration of acid or base; or other fluids. The plant of the invention permits ease and speed in operation by a rapid exchange of exhausted solid without stopping the process. It also allows to operate quickly by a serial process without dismantling reactors of the pilot plant at the end of the experiments. It is also noted that the plant of the invention can operate with different types of biomass, without limitations due to the particle size of the biomass, also allowing the solid collected entirely exhausted. Finally it is noted that the innovations of the invention achieve greatly reduce the time of the extraction process and also manage to eliminate downtime.

Technical problem to be solved and background of the invention

Currently, the lignocellulosic materials belong to the 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 primarily of lignin, cellulose and hemicellulose, associated in a resistant structure whose rupture requires a considerable amount of energy. However, thanks to its differentiated composition, allow to obtain multiple fuels and high value chemicals.

A promising, clean and inexpensive way for depolymerizing hemicellulose into monosaccharides is called hydrothermal hydrolysis process which simply involves treating the biomass with water at different temperatures, or water with a low concentration of acid.

The most efficient way to extract hemicellulose from biomass is the use of systems in the flow, in which reactors are loaded with pellets or powder of biomass, while a continuous flow of liquid (water or acid) is introduced continuously in 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 major problems currently existing installations for the purpose described, is charged and discharged solid material contained in each reactor once is complete extraction process. In fact, the wet biomass swells and compact, making it impossible to remove without stopping the system, without opening it. This implies long idle times. In many cases they particles with dimensions of the order of microns, which presuppose crushing biomass, with consequent energy consumption and pumping the slurry consisting of water and biomass are used, which also means a power consumption added.

Patent with Publication No. WO 2015009986 A2 describes a method for obtaining hemicellulose using water or with acid, through a reactor in flow.

Patent with Publication No. 6022419 US A refers to a reactor in which the volume occupied by the solid (sawdust), continuously decreases by the effect of a spring, pushing it limb.

Patent with Publication No. WO 201 1091044 A1 describes a process for extracting cellulose and hemicellulose of the biomass, with subcritical and supercritical water, through a continuous reactor fed with a slurry of water and biomass. Patent with Publication No. 6228177 US B1 describes a system in series, for the extraction of lignocellulosic material, wherein the reactors are cooled by immersion in cold water.

Also known publishing King SD referring to "The Future of Industrial biorefineries". In: Forum WE, editor; 2010.

DESCRIPTION OF THE INVENTION

In order to achieve the objectives and avoid the drawbacks mentioned in the preceding paragraphs the invention proposes a multibed pilot biomass fractionation plant is to draw and fractionate on bio continuous as polyphenols, beta-glucans, caffeine and biopolymers as hemicellulose from residual lignocellulosic biomasses and no residual of different origins.

Plant biomasses contain many interesting products. Some of these, such as polyphenols contained in the seeds and skins of grapes, beta-glucans present in oats in barley and mushrooms, and especially hemicellulose essential component of plants, and listed in all plant products, can be extracted only with water at different temperatures. The first two mentioned compounds are of great importance in health and human well-being: polyphenols are compounds with antioxidant properties that have aroused great interest in health and prevention of diseases associated with an increase in the processes of cell oxidation (cancer , cardiovascular diseases and neurodegenerative diseases); beta-glucans improve control of blood glucose and lipid levels, such as cholesterol or triglycerides.

Hemicellulose, when isolated from biomass in molecular weights above 3-5 kDa, has unique properties. It can be used to produce films for packaging applications replacing the synthetic plastics, functions as barriers against oxygen penetration; Another important application is the production of aerogels to insulate food products.

Xylose from hemicellulose, for example, can be converted to furfural, which is a precursor used in different fields, such as oil refining, plastics, pharmaceutical and agrochemical. The xylose may also be hydrogenated or enzymatically transformed into xylitol, which is a sweetening agent and is also used for the prevention of dental caries.

The idea of ​​transformation of biomass into energy, materials and chemicals, defines the concept of biorefinery, particularly interesting topic today, taking into account issues related to fossil fuels and derivatives.

Two categories of raw materials dominate the research: first and second generation. First generation products are produced from biomass such as edible starchy or oily plants; second-generation products using biomass waste consisting of non-edible parts of current crops or other non-food sources, such as perennial grasses or algae. These are widely recognized as having a significantly greater potential to replace fossil products (King, 2010).

Lignocellulosic materials belong to the second generation raw materials, and can be obtained from various sources, such as wood waste, agricultural waste or municipal, which do not interfere with crops for direct human consumption. They consist primarily of lignin, cellulose and hemicellulose, associated in a resistant structure whose rupture requires a considerable amount of energy; However, thanks to its differentiated composition, allow to obtain multiple fuels and high value chemicals.

Lignocellulosic biomass can be fractionated into cellulose, hemicellulose and lignin, from which can be produced sugars, fuels, chemicals and materials. From waste processing can produce energy. The plant of the invention offers great improvements in the extraction of hemicellulose, an integral part of biorefinery process. Moreover the plant of the invention includes numerous innovations for the extraction of bioproducts from biomass, and allows:

- continuous extraction of biopolymers and biocomposites from biomass, with subcritical water (up to 16 bar and 200 ° C).

- rapid exchange of exhausted solid without stopping the process.

- Energy saving between 85% and 95% through a system of heat exchange with product and use in the samplings.

- Possibility to operate with different types of biomass, without limitations due to particle size.

- Ease and speed of operation, minimal physical contact with the apparatus.

The pilot plant multibed is applicable to processing industries soluble coffee; however in these industries it is used merely vacuum extractor as tubular structures including those industries are large enough to dislodge the solid exhausted. Instead, pilot plant solid material jams and create serious problems for an extraction operation continuously possible. With the plant of the invention is achieved load biomass in a cartridge that is inserted hot in each reactor, so that a series of valves able to isolate the beds so as to exchange the exhausted biomass without stopping the fractionation process and extraction achieved in the plant of the invention.

The multibed pilot plant of the invention comprises reactors interconnected together by a circuit pipe through which flows a liquid fluid delivered by at least one motor pump; where reactors include some cartridges containing biomass, a liquid inlet fluid traveling through the biomass contained within the cartridges and a liquid outlet fluid containing various substances extracted from biomass housed within cartridges.

The pilot plant of the invention further comprises vertically arranged reactors having the liquid inlet fluid above the cartridge, and the liquid outlet fluid is located in a bottom of the reactors.

At the lower ends of the reactors connected devices opening and closing of said reactors located below the cartridge; wherein the cartridges are introduced into the reactors and removed from the interior of said reactor through the opening and closing devices when placed in an open position.

The pipe circuit comprises leg portions through which flows the liquid fluid directed toward the liquid inlets fluid within the reactor, and a return portions through which flows the liquid fluid when it leaves the reactor; where valves for isolating the reactors independently for exchanging cartridges without stopping the operation of the pilot plant are interleaved in said pipe circuit parts.

Each of the leg portions of the piping circuit includes a first three-way valve and a second valve two-way interleaved in a branch that starts from the reactor inlet.

Each of the parts return piping circuit includes at least a first two-way valve. An output of the first three-way valve connected to a pipe section feeding into the reactor; while another outlet of the first three-way valve feeds an intermediate stretch connecting the first valve with another three-way interleaved elsewhere in circuit flow pipe.

The first two-way valve is interposed in a section of pipe that starts from the reactor outlet and connects said intermediate section.

The plant of the invention includes a needle valve two interleaved positions in an end section of pipe connecting the pipe section the reactor outlet and with a heat exchanger connected to a second three-way valve having a outlet connecting with a first tube for sampling the liquid fluid, and a second output connected to a second tube. A first section of the piping circuit includes initial heat exchangers in combination with a main heater located below such heat exchangers initial.

The pilot plant comprises a multibed pressure valve for regulating the pressure within the reactor; wherein said pressure valve is located in an initial derivation of circuit flow pipe.

The return portion of a corresponding last reactor with the liquid outlet fluid from said last reactor, connected to a shunt feedback opening into an initial region of the part of circuit flow pipe.

Each of the reactors has an additional output which connects a top branch pipe opening into a container; wherein in said bypass pipe is interposed a third two-way valve.

In one embodiment, each of the devices of opening and closing of the reactors comprises a ball valve.

The pilot plant comprises means parachute attached to the opening and closing devices located at the lower ends of the reactors; wherein said paracaíadas devices cushion the fall of the cartridges when removed from inside the reactors.

The reactors are coated homogeneously by means for heating said reactors surround and maintain the temperature resistance.

Each of the reactors of the plant comprising:

- a tubular mesh which is filled with biomass.

- an inner tubular housing having a lower perforated bottom and an open top base; where within said tubular casing inside the tubular mesh is located.

- a tubular outer casing where the cartridge constituted by the inner tubular housing and the tubular mesh is housed.

The tubular mesh comprises two half demountable parts are coupled together through two opposite generatrices which follow a broken path.

The inner tubular housing comprises two separate parts: a first part including the lower perforated base, and a second part which includes a narrowing where the upper open base is located.

The outer tubular casing of each reactor comprises a main body and a lid which closes the main body at its upper end while its lower end connected to the opening and closing device; wherein the lid includes a liquid inlet fluid within the reactor; and wherein the main body includes a liquid outlet and further fluid outlet connecting with the bypass pipe draining of the liquid fluid in the container.

In one embodiment of the invention, the tubular mesh, lower tubular housing and tubular outer housing having a cylindrical configuration and are formed of a metallic material.

Each heat exchanger located in the portion of circuit return pipe, comprising two concentric tubes: outer and inner; wherein the liquid fluid contained in the reactor, cooled by water flowing through the outer tube is discharged from the inner tube. Each of the devices parachute comprises a front plate depending from at least two suspension elements connected to a part of the opening and closing device; wherein said front plate is located below the opening and closing device for receiving the cartridge when the opening and closing device opens.

The pilot plant comprises a first motor-pump used early in the process to fill the reactor before the pipe circuit is opened to carry out the extraction and fractionation continuous solubles residual biomass and no residual. Said first motor pump feeds a clean fluid or liquid contained within a first deposit.

The pilot plant further comprises a second pump and motor that drives the fluid through the liquid piping circuit for carrying out the process of continuous extraction and fractionation of soluble compounds of the residual biomass and no residual. Said second motor-pump feeds a liquid fluid contained within a second reservoir.

The process for fractionating biomass carried out by the pilot plant described multibed comprises the following steps:

- heating the liquid fluid by initial heat exchangers.

- heating the liquid fluid through the main heater.

- introducing the liquid fluid within the reactor above the cartridges;

- heating the reactors by resistors enclosures located around the reactors.

- extracting the liquid fluid within the reactors.

- varying the temperature of fluid removed from the reactors through the heat exchangers.

- change cartridges reactors with new ones without stopping the process.

- taking samples extracted from inside after passing through the heat exchangers through the first fluid tube reactors.

- collecting the extracted from inside after passing through the heat exchangers reactors fluid through the second tubes.

- regulating the pressure within the reactor 1 via the pressure valve.

- channeling of the liquid fluid introduced into the reactors to the containers; wherein when said containers are filled liquid flow into containers is interrupted.

In one embodiment the process comprises an additional step in which the extracted from the last reactor to the initial part of liquid piping circuit fluid is returned.

Hereinafter to provide a better understanding of this specification and forming an integral part thereof, a series of figures in which with an illustrative and nonlimiting character represent the object of the invention is attached. BRIEF DESCRIPTION OF THE FIGURES

Figure 1 shows a view of the pilot multibed for fractionating biomass, plant of the invention. It comprises a set of reactors in combination with other elements to carry out the extraction and fractionation continuous solubles. It is also object of the invention the process to carry out the biomass fractionation.

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 along with a ball valve, 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 parts of the reactor.

Description of an embodiment of the invention

Considering the numbering adopted in the figures, the multibed pilot biomass fractionation plant comprises several reactors 1 intercommunicating vertical arrangement to each other by parts leg through which flows a liquid fluid directed toward a liquid inlets fluid reactors 1, and return portions through which flows the liquid fluid when it leaves the reactor 1; wherein each of the reactors working in series with the other, with the possibility of being excluded a reactor 1 of the other; and wherein said portions of forward and return part of a piping circuit for flowing the liquid fluid.

Each of the reactors 1 comprises:

- a tubular metal mesh 2 formed of two halves 2a, 2b demountable coupled together through two opposite generatrices which follow a broken path; wherein said tubular mesh 2 is filled with biomass.

- an inner tubular casing 3 of stainless steel with a perforated bottom base 4 and a top open base 5; where within said interior tubular housing 3 the tubular mesh 2 is located; and wherein said inner tubular casing 3 comprises two separate parts: a first part 3 including the lower perforated base 4 and a second part 3b including a constriction 6 where the upper open base 5 is located.

- an outer tubular housing 7 made of stainless steel, wherein the cartridge constituted by the inner tubular casing 3 and the tubular mesh 2. Said stays outer tubular housing 7 comprises a main body 7a and a lid 7b to close the main body on the 7th for its upper end while its lower end connected with a ball valve 9. in the embodiment shown in the figures, the tubular mesh 2 lower tubular casing 3 and the outer tubular housing 7 has a cylindrical configuration.

With this described arrangement, the cartridge assembly is inserted from below into the outer tubular housing 7 through the ball valve 9 when in the open position until it is fully inserted within said outer tubular housing 7.

At this point the ball valve 9 is closed and the end of extraction by passing a liquid fluid inside the reactor 1, it proceeds to the opening of the ball valve 9 fall down by gravity the cartridge is removed out so that the cartridge outlet is damped by means of a parachute 10 located in the outlet area of ​​the ball valve 9.

A constant flow of water (or other suitable liquid fluid) enters through an inlet 1 1 located at the top of each reactor 1 to stroke down within said reactor 1 until it emerges from an outlet 12 located at the bottom of reactor 1; where the inlet 11 is located at the top 7b of the outer tubular housing 7 and the outlet 12 is located at a bottom of the main body 7a said outer tubular housing 7. The liquid flow outlet may move to the next reactor 1, or may be deflected in order to exclude the following reactor 1 and passed to the next reactor 1. Thus the biomass can be discharged (through the opening of the ball valve 9 and the quick removal of the cartridge ) reactor 1 wherein the extraction process is completed, and other reactor 1 can be loaded with another cartridge, then deflected in the reactor 1 liquid flow to continue the extraction process. The plant of the invention allows rapid and continuous operation without stops.

Another important feature of the plant of the invention is the adjustment of the water temperature and control of energy. To do this, before entering the reactors 1, the water passes through a primary heater 13 comprises a spiral coil wound around a metal solid body; wherein said spiral coil is covered by an electrical resistance clamp.

The water then enters the reactor 1, which are coated homogeneously with a resistor 14 surround clamp. After leaving the reactor 1, the liquid fluid enters a heat exchanger 15 concentric tubes. In the outdoor flowing water supply of the plant, which is preheated via a heat exchanger initial 16 and then passes to the main heater 13 described above. The whole system is insulated with a layer of glass wool covered with aluminum foil. The total heat savings is 85% and saving cooling is close to 100%.

Each reactor 1 may be flushed with hot liquid pressurized fluid before removing the cartridge constituted by the tubular mesh 2 and inner tubular housing 3. Between each pair of reactors adjacent one heat exchanger 15 with concentric tubes is located: outside and inside; wherein 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 liquid fluid biomass.

Depending on the compound to be extracted from the reactors, different temperatures are necessary.

Extracting polyphenols requires a temperature between 60 and 80 ° C; extraction betaglucans around 100 ° C; while extraction of hemicellulose requires temperatures between January 10 and 210 ° C. Therefore, an effective temperature control, which is performed by means of PID controller devices is necessary.

To reach temperatures above 100 ° C, it is also necessary to increase the pressure within the reactor 1, which is regulated through a pressure valve 17 located in an initial bypass circuit 18 of the plant pipes.

The plant also includes safety valves in each reactor 1 avoiding any overpressure. a thermostat to prevent overheating of the bulk metal body main heater 13 is also included.

For the extraction operation is continued, it is necessary to quickly download reactor 1. As the plant system of the invention is under pressure, a sudden opening of the ball valve 9 could cause leakage of superheated steam. Therefore, between one reactor and another is placed adjacent the corresponding heat exchanger 15 with concentric tubes: outer and inner.

As it described above, since the inner tube the liquid contained in the reactor 1 after the extraction operation is discharged, and the outer tube flowing cold water then fed to the plant of the invention.

Early in the process, the biomass is introduced into the tubular mesh 2, which can be opened longitudinally, and which is inserted between the two 3a, 3b portions of the inner 3. tubular housing The first part 3 is open at the upper end and the lower end has the lower perforated base 4 with holes diameter between 5 mm and 0.5 mm. As stated earlier, the assembly of the tubular mesh 2 and the inner tubular housing 3 is inserted through the ball valve 9 within the outer tubular housing 7 closed by the top end by the cap 8 which is you can be removed in case the reactor 1 jamming.

The size of the biomass particles loaded in reactor 1, must be greater than the size of the diameter of the holes of the lower perforated base 4 of the inner tubular housing 3, which functions as a filter preventing solid biomass is removed from bed and pulled through the various elements of the plant of the invention.

In one embodiment as shown in Figures 2 and 3, the plant of the invention comprises an operating unit of reactor 1 which is carried out the process for fractionating biomass.

Instead, in Figure 1, a plant that includes several units connected reactors, which can operate in series with each other, or separately, and which also it performs the process for fractionating biomass shown.

Once a reactor 1 is loaded with biomass, as described above, the cartridge is pushed until it comes completely, and then the ball valve 9 located below the cartridge closes. At this time, the reactor 1 with water, driven by a first motor-pump 19, ensuring that the liquid entering the reactor 1 and does not escape through the pipe loop is filled.

For this reason, each reactor 1 from the rest of the pilot plant system is isolated by closing a first two-way valve 20 and a second needle valve 21 located at the outlet of each reactor 1. A second valve also opens 22 two-way valve 23 and a first three-way, is moved so that the water from only one reactor 1, and in the segment of pipe between the reactor and said first three-way valve 23. The first three-way valve 23 may divert the flow to the next reactor 1 or to the next first valve 23 three-way, avoiding the reactor 1 above.

A third valve 24 of two-way connected to an additional output top 25 of each reactor 1 is kept open until it is found that a container 26 begins to fill with fluid flow through a bypass pipe that starts from said third valve 24 and flows into the container 26. then the two-way valves 22 and 24 are closed, and the first motor-pump 19 is switched off the flow of liquid fluid to the reactor 1. in this situation, the biomass contained within the reactor 1 is completely immersed in the liquid fluid, and the reactor 1 is isolated from the pilot plant system.

The reactor 1 is heated homogeneously by envelopes resistors 14 to a temperature slightly lower than the minimum temperature needed to start the extraction of the compound to be extracted.

Hemicellulose extracted starts at temperatures above 100 ° C; so that if said compound is decided extract hemicellulose preheat the reactor 1 and wait for the reactor 1 reaches temperatures above 100 ° C. A second motor-pump 27 is activated to drive the flow of liquid which previously passes through exchangers initial heat 16, functioning as a cooling liquid of other hot liquid exiting the system, while obtaining a first preheating . Consecutively gets further preheating by the main heater 13 to a higher temperature at which it is required to operate; following after the liquid fluid toward the first valve 23 three-way.

As stated earlier, in one embodiment, said first three-way valve 23 is still located in a position in which fluid flow is diverted to the next first valve 23 three-way, and not to the reactor 1.

When the flow reaches the required temperature, the reactor temperature is raised to the conditions with which it is to operate; adjusting the first valve 23 three-way, so that the flow of liquid entering the reactor 1, while the first valve 20 opens two-way for the liquid to exit the reactor 1. At this time begins the extraction of soluble compounds from the biomass in the reactor 1: the flow of liquid entering the reactor 1, passes through the biomass bed, extracted soluble compounds, and leaves the reactor.

The process described so far basically refers to operation of a single reactor unit 1.

The flow of liquid exiting the reactor 1 reaches another first valve 23 three-way, so that acting on the first valve 23 three-way can direct the flow to the next reactor 1 or to the next first valve 23 three-way . This operation can be repeated for each reactor unit in the pilot plant system. Thus, each reactor 1 can be integrated in the extraction process, or may be omitted. After exiting the last reactor 1 used in the system of the pilot plant, the hot liquid stream is returned and enters the inside of initial heat exchangers 16 transferring heat to liquid fed into the system. The liquid outlet, thus cooled, and depressurized through the pressure valve 17, and finally leaves the system. The pressure valve 17 regulates the pressure of the entire exhaust system, so that when it is desired to stop the reaction in reactor 1, the liquid flow is diverted, blocking the supply to the reactor unit 1 corresponding to be isolated from system.

For this, the first three-way valve 23 preceding the respective reactor 1 and the first two-way valve 20 placed at the exit of said reactor 1, thus excluding the corresponding reactor 1 is closed system is rotated. The liquid flow can be directed to the reactor unit 1 subsequent (loaded with a cartridge biomass, as explained above), or can be directed to the first valve 23 three following ways, which in turn can direct the flow.

The needle valve 21 has an outlet opening into the heat exchanger 15, so that when said needle valve 21 opens, the liquid contained in the reactor 1 passes to heat exchanger 15 and cooled by another fluid flowing in the outdoor heat exchanger 15. Thus, the pressurized liquid contained within the reactor is not vaporized during the opening of the needle valve 15, and exits as a normal liquid without pressure.

This system allows the pilot plant reactor completely empty each liquid, once the extraction process is terminated.

On leaving the heat exchanger 15 a second valve 28 three-way allows direct the liquid exiting into a first tube 29 shorter to take a sample of the product, or to a 30 second longest tube connected is connected to a system drain.

After emptying the reactor liquid 1, the ball valve 9 is opened below the reactor 1, so that the cartridge containing the exhausted biomass, fall into the parachute device 10. In this situation, the cartridge can be removed and open, so that the tubular bad 2 is extracted from within the inner tubular housing 3 and then the tubular net 2 is opened longitudinally so that it can collect all the biomass in the solid state. When a reactor operation ends, and the cartridge, another container cartridge fresh biomass can refresh quickly restarting the extraction process in the new mounted cartridge is removed.

The return portion of the last reactor 1 corresponding to the liquid outlet fluid from said last reactor 1, connects to a shunt feedback 8 opening into an initial region of the part of circuit flow pipe.

The first pumping unit 19 is used early in the process to fill the reactor 1 before the pipe circuit is opened to carry out the extraction and fractionation continuous solubles residual biomass and no residual. Said first motor pump 19 feeds a clean fluid or liquid, contained within a first tank 31.

Instead the second motor-pump 27 drives fluid through the liquid piping circuit for carrying out the process of continuous extraction and fractionation of soluble compounds of the residual biomass and no residual. Said second motor-pump 27 feeds a liquid fluid contained within a second reservoir 32.

Therefore the two motor-pumps 19, 27 are fed independently of fluids contained within fluid containers 31, 32; in one embodiment of the invention said fluid liquids are water.

Each of the devices parachute 10 comprises a metal front plate 10a hanging two suspension elements connected to a portion 10b of the ball valve 9; wherein said front plate 10a is located below said ball valve 9. In one embodiment of the invention the suspension elements comprise chains 10b and in another embodiment comprise for example tie rods. With this arrangement described, the front plate 10a can be moved forward or backward to allow the inlet and outlet of the cartridge. Upon removal of the cartridge, the front plate 10a is positioned just below the ball valve 9 for receiving the cartridge falls down by gravity directly on said front plate 10a.

Claims

What is claimed
1. - multibed biomass fractionation pilot plant, comprising reactors interconnected together by a circuit pipe through which flows a liquid fluid delivered by at least one motor pump; where reactors include some cartridges containing biomass, a liquid inlet fluid traveling through the biomass contained within the cartridges and a liquid outlet fluid containing various substances extracted from biomass housed within the cartridge; characterized in that:
- comprises reactors (1) in a vertical arrangement with the liquid inlet fluid over the cartridges and fluid liquid outlet is located in a lower part of the reactor (1);
- at the lower ends of the reactors (1) connected devices opening and closing of said reactors (1) located below the cartridge; wherein the cartridges are introduced into the reactors (1) and removed from the interior of said reactor through the opening and closing devices when placed in an open position;
- the pipe loop comprises parts leg through which flows the liquid fluid directed toward the liquid inlets fluid within the reactors (1), and a return portions through which flows the liquid fluid when exiting reactors 1 ; where valves for isolating the reactors independently (1) for exchanging cartridges without stopping the operation of the pilot plant are interleaved in said pipe circuit parts.
2. - multibed pilot for fractionating biomass, according to claim 1, characterized in that plant:
- each of the leg portions of piping circuit includes a first valve (23) and a second three-way valve (22) two-way interleaved in a branch that starts from the reactor inlet;
- each of the parts return piping circuit includes at least a first valve (20) two-way;
where,
- an output of the first valve (23) three-way connected with a pipe section which feeds the reactor (1); while another outlet of the first valve (23) three-way feed an intermediate section that connects with another first valve (23) three-way interleaved elsewhere in circuit flow pipe;
- the first valve (20) two-way interleaved is a pipe section that starts from the outlet of reactor (1) and connects said intermediate section.
3. multibed pilot for fractionating biomass, according to claim 1, characterized in that plant includes a needle valve (21) interleaved two positions at one end section of pipe connecting to the pipe section the reactor outlet ( 1) and a heat exchanger (15) which connects with a second valve (28) three-way having an output that connects to a first tube (29) for sampling the liquid fluid, and a second output connected to a second tube (30).
4.- multibed pilot biomass fractionation plant according to claim 2, wherein a first section of the piping circuit includes initial heat exchangers (16) in combination with a main heater (13) located below the said exchangers initial heat (16).
5. multibed pilot biomass fractionation plant according to claim 1, characterized by comprising a pressure valve (17) to regulate the pressure inside the reactors (1); wherein said pressure valve (17) is located in an initial branch (18) of the leg part of the piping circuit.
6. multibed pilot biomass fractionation according to claim 1, characterized in that the corresponding return portion of a last reactor (1) with the liquid outlet fluid from said last reactor (1), Plant connects with a bypass feedback (8) opening into an initial region of the part of circuit flow pipe.
7. - multibed pilot biomass fractionation according to claim 1, characterized in that each of the reactors (1) has an additional output upper (25) which connects a branch pipe opening into a container (26) Plant; wherein in said bypass pipe is interposed a third valve (24) two-way.
8. - multibed pilot biomass fractionation according to claim 1, characterized in that each of the devices of opening and closing of the reactors (1) comprises a ball valve (9) Ground.
9. multibed pilot biomass fractionation plant according to claim 1, characterized by comprising devices parachute (10) attached to the opening and closing devices located at the lower ends of the reactors (1); wherein said paracaíadas devices (10) cushion the fall of the cartridges when removed from inside the reactor (1).
10. multibed pilot biomass fractionation plant according to claim 1, characterized in that the reactors (1) are coated homogeneously with a wraparound resistors (14) for heating said reactors (1) and maintain temperature.
11.- multibed pilot biomass fractionation plant according to claim 1, wherein each of the reactors (1) comprises:
- a tubular mesh (2) which is filled with biomass;
- an inner tubular housing (3) it is having a perforated lower base (4) and an open upper base (5); where within said interior tubular housing (3) the tubular mesh (2) is located;
- an outer tubular housing (7) where the cartridge constituted by the inner tubular casing (3) and the tubular mesh (2) is housed.
12. - multibed pilot for fractionating biomass, according to claim 1 1, characterized in that the tubular mesh (2) comprises two halves (2a, 2b) which is detachable coupled together through two opposite generatrices that follow one plant broken trajectory.
- 13. multibed pilot for fractionating biomass, according to claim 1 1, characterized in that the inner tubular casing (3) comprises two separate parts plant: a first part (3a) including the lower perforated base (4), and second part (3b) includes a constriction (6) where the top open base (5) is located.
14. - multibed pilot biomass fractionation according to claims 7 and 11, characterized in that the plant tubular outer housing (7) of each reactor
(1) comprises a main body (7a) and a cover (7b) which closes the main body (7a) at its upper end while its lower end connected to the opening and closing device; wherein the cover (7b) includes an inlet (11) of liquid fluid in the reactor (1); and wherein the main body (7a) includes an outlet (12) of liquid fluid and the additional outlet (25) connecting the bypass pipe draining of the liquid fluid in the container (26).
15. - multibed pilot for fractionating biomass, according to claim 1 1, characterized in that the tubular mesh (2), the lower tubular housing (3) and tubular outer housing (7) have a cylindrical configuration and are formed of a material Planta metal.
- 16. multibed pilot for fractionating biomass, according to claim 3, characterized in that each heat exchanger (15) located in the portion of circuit return pipe, comprising two concentric tubes Plant: exterior and interior; wherein the liquid fluid contained in the reactor (1), cooled by water flowing through the outer tube is discharged from the inner tube.
17. - multibed pilot biomass fractionation according to claim 9, wherein each of the devices parachute (10) comprises a front plate (10a) depending from at least two suspension elements (10b) connected to ground a part of the opening and closing device; wherein said front plate (10a) is located below the opening and closing device.
18. - multibed pilot biomass fractionation according to claim 1, characterized by plant comprising:
- a first motor-pump (19) to fill the reactors (1); wherein said first pump motorcycle (19) is fed from a liquid fluid contained within a first reservoir (31);
- a second motor-pump (27) that drives the liquid fluid through the piping circuit; wherein said second motor-pump (27) feeding a liquid fluid contained within a second reservoir (32).
19. - Process for fractionating biomass, carried out by the pilot plant multibed described in the preceding claims 1 to 18, characterized by comprising the steps:
- heating the liquid fluid by initial heat exchangers (16);
- heating the liquid fluid through the main heater (13);
- introducing the liquid fluid within the reactors (1) above cartridges;
- heating the reactor (1) via resistors envelopes (14) arranged around the reactors (1);
- extracting the liquid fluid within the reactors (1); - varying the temperature of fluid removed from the reactor (1) through heat exchangers (15);
- changing cartridges reactor (1) by new ones without stopping the process;
- sampling the extracted fluid within after passing through the heat exchangers (15) through the first tubes (29) reactors;
- collecting the extracted from inside the reactor (1) after passing through the heat exchangers (15) fluid through the second tubes (30);
- regulating the pressure within the reactor (1) through the pressure valve;
- channeling of the liquid fluid introduced into the reactor (1) to the containers (26); wherein when said containers (26) filled liquid flow into containers (26) is interrupted.
20.- Process for fractionating biomass, according to claim 19, characterized by comprising an additional step of returning the liquid fluid removed from the last reactor (1) to 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 WO2018050941A1 (en)

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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

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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