FI20185854A1 - A method and an apparatus for increasing concentration of soluble carbohyrate containing fraction, a soluble carbohyrate containing fraction, a solid fraction and their use - Google Patents

Abstract

The invention relates to a method and an apparatus for producing a soluble carbohydrate containing fraction (10), in which lignocellulose material (3) formed by treating plant based raw material (1) is conducted into a separation stage (4). The method comprises at least one solid-liquid separation stage (4) for separating a soluble carbohydrate containing fraction (10) and/or a washing filtrate (12) from lignocellulose material (3), and at least a part of the soluble carbohydrate containing fraction (10) and/or the washing filtrate (12) is recirculated to the lignocellulose material (3) for increasing concentration of the soluble carbohydrate containing fraction, and solids (11) and at least a part of the soluble carbohydrate containing fraction (10) are supplied out from the separation stage. Further, the invention relates to the soluble carbohydrate containing fraction and the solid fraction, and their uses.

Description

A METHOD AND AN APPARATUS FOR INCREASING CONCENTRATION OF SOLUBLE CARBOHYRATE CONTAINING FRACTION, A SOLUBLE CARBOHYRATE CONTAINING FRACTION, A SOLID FRACTION AND THEIR USE

FIELD OF THE INVENTION

The invention relates to a method and apparatus for producing a soluble carbohydrate containing fraction and a solid fraction. Further, the invention relates to a soluble carbohydrate containing fraction and its use. Further, the invention relates to a solid fraction and its use.

BACKGROUND OF THE INVENTION

Known from prior art is different methods for forming carbohydrates from different raw materials such as biomass. Many bio-refinery processes, e.g. hydrolysis, generate lignin and sugars after treatment of the biomass.

OBJECTIVE OF THE INVENTION

The objective of the invention is to disclose a novel method for producing a soluble carbohydrate containing fraction with high concentration. Another objective of the invention is to produce a soluble carbohydrate containing fraction with increased concentration and with improved recovery. Another objective of the invention is to improve the biomass fraction for producing an improved, concentrated liquid fraction consisting of soluble carbohydrates with high recovery and a soluble material free solid fraction.

SUMMARY OF THE INVENTION

The Method For Increasing Concentration Of A Soluble Carbohydrate Containing Fraction According To The Present Invention 1.

The apparatus for increasing the concentration of a soluble carbohydrate containing fraction according to the present invention 13.

The soluble carbohydrate containing fraction according to the present invention is characterized by what is stated in the claim 17.

The solid fraction according to the present invention is characterized by what is presented in the claim 19.

The use of the soluble carbohydrate containing fraction according to the present invention is characterized by what is presented in the claim 23.

The use of the solid fraction according to the present invention is characterized by what is presented in the claim 24.

BRIEF DESCRIPTION OF THE DRAWINGS

The accompanying drawings which are included to provide a further understanding of the invention and to provide a part of this Specification illustrate some embodiments of the invention and together with the description help to explain the principles of the invention. In the drawings:

Fig. 1 is a flow chart illustration of a method according to one embodiment of the present invention,

Figure 2 is a flow chart illustration of a method according to another embodiment of the present invention,

Fig. 3 is a flow chart illustration of a method according to another embodiment of the present invention,

Figure 4 is a flow chart illustration of a method according to another embodiment of the present invention

Fig. 5 is a flow chart illustration of a method according to another embodiment of the present invention,

Fig. 6 is a flow chart illustration of a method according to another embodiment of the present invention,

Fig. 7 is a flow chart illustration of a method according to another embodiment of the present invention,

Fig. 8 shows results from one example carried out according to one method of present invention,

Fig. 9 shows results from one example carried out according to one method of present invention, and

Fig. 10 shows results from one example carried out according to one method of present invention.

DETAILED DESCRIPTION OF THE INVENTION

The invention relates to a method for increasing the concentration of a liquid fraction consisting of a soluble carbohydrate, such as a soluble carbohydrate containing fraction, in which the lignocellulose material (3) is formed by treating the plant based raw material (1). , 6). In the method of the present invention, the method comprises at least one solid-liquid separation step (4,6) for separating a soluble carbohydrate containing fraction (10) and / or washing filtrate (12) from lignocellulose material (3). The separation stage consists of one or more separation steps. At least part of the cellular carbohydrate containing fraction (10) and / or the washing filtrate (12) is recirculated to the lignocellulose material (3), preferably before the desired separation step (4.6) ), for increasing the concentration of the soluble carbohydrate containing fraction. Solids (11) and at least part of the soluble carbohydrate containing fraction (10) are supplied from the separation stage. In one embodiment, at least part of the washing filtrate (12) is supplied from the separation stage.

One embodiment of the method of the present invention is shown in Figure 1. Another embodiment of the method of the present invention is shown in Figure 2. Another embodiment of the method of the present invention is shown in Figure 3. Another embodiment of the present invention is shown in Fig. 4. Another embodiment of the present invention is shown in Fig. 5. Another embodiment of the present invention is shown in Fig. 6. method of the present invention is shown in Figure 7.

The apparatus of the present invention comprises at least one solid-liquid separation device (4,6) into which lignocellulose material (3) is formed by treating plant based raw material (1) and is conducted in which a soluble carbohydrate containing fraction (10) and / or a washing filtrate (12) are separated from lignocellulose material (3). Further, the apparatus comprises at least one feeding device, such as a pump, for feeding the lignocellulose material (3) into the separation device (4,6). Further, the apparatus comprises at least one recirculation device for recirculating at least a portion of the soluble carbohydrate containing fraction (10) and / or washing filtrate (12) to the lignocellulose material (3), preferably before the desired separation device or separation step, for increasing the concentration of the soluble carbohydrate-containing fraction. Further, the apparatus comprises means, such as discharge means or outlet means, for supplying solids (11) and at least a portion of the soluble carbohydrate containing fraction (10) out of the apparatus. In one embodiment, the apparatus comprises means for supplying at least a portion of the washing filtrate (12) out of the apparatus.

The invention is based on a solid-liquid separation. Further, the invention is based on a recirculation of the filtrates containing preferably sugars, such as a soluble carbohydrate containing fraction and / or washing filtrate, in order to increase the concentration of the soluble carbohydrate containing fraction. In the invention, the sugar content of the soluble carbohydrate containing fraction can be increased by means of the recirculation of the filtrates in various applications. Simultaneously, the recovery of the liquid soluble carbohydrate containing fraction can be increased and more pure solid fraction formed solids can be formed. Further, carbohydrate content and purity of solids can be increased by means of the present invention. Further, if the washing filtrate is formed so it can be utilized in the process. In one embodiment, a small amount of washing is used and thus the concentration of soluble compounds can be further increased. In one embodiment, a replacement washing is used which leads to a further increase in the concentration of the soluble compounds and an increase in the purity of the solid fraction.

In this context, a washing filtrate means a dilute filtrate from a washing step in which the lignocellulose material is washed. In this context, a soluble carbohydrate containing fraction means a soluble carbohydrate containing filtrate, preferably with a high concentration separated from the lignocellulose material. In a preferred embodiment, the washing filtrate and the soluble carbohydrate containing fraction include carbohydrates, preferably C5 sugars (Ο5Η10Ο5 or (C5 (H2O) n) · The soluble carbohydrate containing fraction may include carbohydrates, such as monosaccharides (C6H12O6 or C5H10O5), disaccharides (Ci2H220h), oligosaccharides and / or polysaccharides ((CgHxo05) n or (CsHgOJn) · Preferably, the soluble carbohydrate containing fraction comprises soluble C5 carbohydrates (Ο5Η10Ο5 or C5 (H2O) n) and other carbohydrates. fraction may also form other carbohydrates, and preferably solid carbohydrates (C6H12O6 or C6 (H2O) n) · The solids may also comprise other carbohydrates and other components.

In this context, plant based raw material means any plant based raw material, e.g. wood based raw material. The plant-based raw material includes lignin, cellulose and hemicellulose. In one embodiment, plant based raw material is selected from group consisting of wood based raw material, wood, lignocellulose biomass, agricultural residues, bagasse based material, sugarcane bagasse, corn based material, corn stover, wheat straw, rice straw, woody biomass, woody perennials, vascular plants and their mixtures and their combinations. In one embodiment, the plant-based raw material is a wood-based raw material or a mixture comprising a wood-based material. In one embodiment, the plant-based raw material comprises plant pieces, e.g. wood pieces.

In this context, lignocellulose material refers to any lignocellulose material that has been formed by treatment, such as pre-treatment, from a plant-based raw material by means of a suitable treatment method in one or more steps. In one embodiment, the lignocellulose material contains carbohydrates and lignin. Preferably, the carbohydrates have Cn (H2O) n or Cn (H2O) ni · The carbohydrates can consist of monosaccharides (C6H12O6 or Ο5Η10Ο5), disaccharides (Ci2H220n), oligosaccharides and / or polysaccharides ((C6H10O5) n or (CsHgOJ, the lignocellulose material includes carbohydrates, such as soluble C5 carbohydrates (Ο5Η10Ο5 or C5 (H2O) n) and solid C6 carbohydrates (C6H12O6 or C6 (H2O) n) · The lignocellulose material may contain one or more lignocellulose material components. the lignocellulose material (3) is formed from the plant-based raw material (1) and is treated in one or more treatment step (2,5). , the lignocellulose material is formed or treated by treatment, preferably by pretreatment, selected from the group consisting of physical treatment, such as milling, extrusion, microwave treatment, ultrasound treatment and freeze treatment, chemical tre atment, such as acid treatment, alkaline treatment, ionic liquid treatment, organosolv treatment and ozonolysis, physico-chemical treatment, such as steam explosion treatment, ammonia fiber explosion treatment, C02 explosion treatment, liquid hot water treatment and wet oxidation, biological treatment and their combinations. Preferably, the plant-based raw material is treated to dissolve hemi-cellulose. In one embodiment, the lignocellulose material is formed or treated by the hydrolysis, e.g. acid hydrolysis, autohydrolysis, thermal hydrolysis, enzymatic hydrolysis, supercritical hydrolysis, and / or sub-critical hydrolysis, in which at least part of the lignin is separated from the raw material in connection with the hydrolysis. In one embodiment, the lignocellulose is formed or treated by the steam explosion, in which the hemicelluloses are treated and in which at least part of the polysaccharides are de-graded into monosaccharides and oligosaccharides. In one embodiment, the lignocellulose material is formed or treated by the hydrolysis and by the steam explosion in one or more steps. In one embodiment, the lignocellulose material is formed or treated by the Catalytic pretreatment, e.g. by using acid or base as Catalyst. In the pretreatment process, the plant-based raw material enters the Reactor unit where the pretreatment takes its place. The lignocellulose material can be treated with means of one or more treatments. The treated lignocellulose material can then blown to a Blow-tank. Further, the lignocellulose material can be dewatered, e.g. by dewatering presses in two stages. The dewatering makes possible separate sugar based Streams. In one embodiment, the lignocellulose material consists of fine solid particles. By means of fine particle size high yields and low amount of degradation can be achieved in the process. Preferably, fine solid particles are fiber-like or indefinable particles smaller than 0.2 mm, or they are particles that are small enough to pass through the Bauer McNett 200-mesh screen. The particle size of the lignocellulose material can be measured, e.g. with an optical measurement device such as the Metso FS5, or a laser diffraction method such as the Coulter LS230. The values for particle size are dependent on the method and thus values from Metso FS5 and Coulter LS230 cannot be directly compared. Particle size of solid particles can be defined based on ISO 16065-N or TAPPI T271. The pretreatment process decreases the particle size and fiber length of the original wood fiber, which can be defined by separating the fibers by cooking the wood in e.g. sulphate process or maceration. The sulphate process is the resultant fiber length of about 80% of the one after the maceration.

In one embodiment, the dry matter content of the lignocellulose material is 20 - 80% by weight after the pretreatment. The dry matter content was determined at 45 ° C by means of evaporation. When the determination of the dry matter content is made at a temperature of 45 ° C so also small-molecular organic compounds remain in the mass during the drying of the determination. In one determination, the determination of the dry matter content can be made, at least partially or as applied, by the National Renewable Energy Laboratory (NREL), Laboratory Analytical Procedures for Standard Biomass Analysis (NREL / TR) -510-48087 (revised July 2011). In one embodiment, the lignocellulose material is diluted with liquid, preferably with water, or steam to form the lignocellulose material feed to the separation stage. In one embodiment, the feed concentration of the lignocellulose material is 2 to 60% by weight, preferably 5 to 30% by weight, more preferably 10 to 20% by weight, into a solid-liquid separation step. If the feed concentration of the lignocellulose material is low so then the size of the device increases. Preferably, the washing filtrate and / or soluble carbohydrate containing fraction which is recirculated to the lignocellulose material is used in the dilution of the lignocellulose material.

In one embodiment, the lignocellulose material is fed by means of a pump, e.g. a mono pump or a piston pump or other suitable pump, into the solid-liquid separation stage. Selection of the pump is based on e.g. feed concentration and / or viscosity of the lignocellulose material.

The solid-liquid separation step may comprise one or more separation steps. In one embodiment, the solid-liquid separation is carried out in one or more separation steps in the separation stage. In one embodiment, the solid-liquid separation step comprises more than one sequential separation step. In one embodiment, the solid-liquid separation step comprises different procedures which may be done in separate separation steps. Alternatively, more than one procedure is done in one process step.

In one embodiment, the separation of the soluble carbohydrate containing fraction and the washing filtrate is carried out in the same separation step. In one embodiment, the separation of the soluble carbohydrate containing fraction and the washing filtrate is carried out in the separate separation steps. In one embodiment, the soluble carbohydrate containing fraction is separated in one step. In one embodiment, the soluble carbohydrate containing fraction may be separated at the first step in a two-step process or a multi-step process. In one embodiment, the soluble carbohydrate containing fraction may be separated at the last step in a two-step process or a multi-step process. In one embodiment, the soluble carbohydrate containing fraction may be separated between the first and last steps. Alternatively, the soluble carbohydrate containing fraction may be separated in more than one step. In one embodiment, a fraction of the soluble carbohydrate or a fraction of the soluble carbohydrate may be separated in connection with the pretreatment process in which the lignocellulose material is formed and / or treated. In one operation, the washing filtrate is separated in one step. In one embodiment, the washing filtrate is separated in more than one step. In one embodiment, the soluble carbohydrate containing fraction and / or washing filtrate are separated in each separation step.

In one embodiment, the washing filtrate is not separated from the lignocellulose material (3). Then, only a soluble carbohydrate containing fraction (10) is separated from the lignocellulose material (3). In one operation, the washing step is not carried out, and the washing filtrate is not formed. Then, only a soluble carbohydrate containing fraction (10) is separated from the lignocellulose material (3).

In one embodiment, the method consists of more than one separation stages. In one embodiment, the method consists of more than one sequential separation stages.

In one embodiment, the apparatus comprises more than one separation devices. In one embodiment, the solid-liquid separation stage comprises at least one separation device. In one embodiment, the solid-liquid separation stage comprises more than one separation device. In one embodiment, one or more separation steps can be done in the same separation device. In one embodiment, the separation device comprises one or more separation step, e.g. separation segment.

In one, the separation device is based on a countercurrent washing. In one embodiment, the separation device is selected from the group consisting of filtration device, centrifugal device, and their combinations. In one embodiment, the separation device is selected from the group consisting of pressure filtration device, vacuum filtration device, filtration device based on underpressure, filtration device based on overpressure, filter press, other suitable press, centrifugal device and their combinations. In one embodiment, the separation device is a pressure filtration device, a vacuum filtration device, a filtration device based on an overpressure or a filtration device based on an overpressure. Alternatively, the separation device can be another washing device in which low amount of washing water is used and washing is done in high dry matter content. Then good recovery can be achieved.

Preferably, the solid-liquid separation step comprises the separation of the soluble carbohydrate-containing fraction and / or the washing filtrate from the lignocellulose material. In one embodiment, the soluble carbohydrate containing fraction and / or the washing filtrate are separated from the lignocellulose material by means of filtration, centrifugal treatment or their combinations. In one, the filtration is carried out by pressure, underpressure or overpressure.

In one embodiment, the solid-liquid separation step comprises the filtration in which the soluble carbohydrate-containing fraction is separated in the liquid form and the solid cake is formed. Preferably, pressure is used in the filtration. In one embodiment, the liquid is separated by a pressure difference, such as by means of vacuum or overpressure. In one embodiment, the solid-liquid separation stage comprises a wash in which a displacement of the lignocellulose material is carried out with a small amount of clean water in order to remove the majority of the sugars, inhibitors and other soluble compounds from the solid lignocellulose material. provide high recovery of soluble compounds. Preferably, ratio of washing water to solid is below 6, preferably below 3 and more preferably below 1.5. In one embodiment, the solid-liquid separation stage comprises filtration and washing. In one embodiment, filtration and washing are carried out in a static chamber, preferably in a non-moving chamber. In one operation, the filtration and washing is carried out in one device under pressure without mixing between the filtration and washing. Preferably, said separation device comprises filtration and washing in a vertical or horizontal plane, not in an inclined plan. High concentration and recovery of soluble material in the liquid phase can be achieved with a small amount of clean water and a solid fraction without soluble compounds can be achieved.

In one embodiment, the separation stage comprises the extraction, liquid separation and washing.

In one embodiment, the soluble carbohydrate containing fraction and / or the washing filtrate are separated from the lignocellulose material by means of pressure filtration. In one embodiment, the apparatus comprises at least one pressure filtration device as a solid-liquid separation device. In one embodiment, the solid-liquid separation stage comprises one pressure filtration device. In one embodiment, the solid-liquid separation stage comprises more than one pressure filtration device. In a preferred embodiment, the washing in the pressure filtration device is based on the displacement of the liquid. In one embodiment, the pressure filtration comprises pumping step, pressing, washing step, pressing and removing of a cake. In the pumping step, the solid cake is formed and pressed. Preferably, in the pumping step, the chamber for the pressure filtration device is filled, and the pre-pressing is made. In one turn, the Air Blow is made after the pumping step or after the first pressing step to further remove the liquid from the cake. Preferably, the soluble carbohydrate containing fraction is separated in the connection with the pumping step. In the washing step, the washing water is pressed through the cake and the cake is pressed and preferably dewatered. In the washing step, the liquid of the cake can be displaced by water. In one turn, the air blow is made in the washing step to further remove the liquid from the cake. The washing filtrate is separated by pressing in the connection with the washing step. The dewatered solid cake is removed from the pressure filtrate device. Preferably, the dewatered solid cake forms a solid fraction.

An advantage of pressure filtration is that all separation steps can be carried out by one device.

In different separation stages, the separation can be carried out by means of similar or different separation methods or separation devices.

In one, an amount of the washing filtrate is optimized by adjusting the washing water ratio. In one, the ratio of washing water to solid composition is 1: 1 to 6: 1, preferably, 1: 1 to 5: 1, more preferable 1: 1 to 4: 1, now preferable 1: 1 to 3: 1, in the washing. Preferably, the water balance is optimized in the method of the present invention.

In one embodiment, at least part of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated to the lignocellulose material before the separation step. In one embodiment, at least a fraction of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated to the desired lignocellulose material prior to the desired separation step, e.g. before the first separation step or between two separation steps. In one embodiment, at least part of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated back to the lignocellulose material which is fed in the same separation stage. In one embodiment, at least part of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated to the lignocellulose material which is fed to the next separation step or the next separation step. In one embodiment, at least a fraction of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated by supplying into a Blow tank, into an entry side of a solid-liquid separation device, into an entry side of a feeding device or into a first step of the solid-liquid separation device, eg into the first step of pressure filtration de- vice. In one embodiment, at least a portion of the washing filtrate and / or fraction containing the carbohydrate is recirculated back to the desired separation step, e.g. segment, of the separation device. In one embodiment, at least a fraction of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated back to the previous separation step, e.g. segment, of the separation device. In one embodiment, at least a fraction of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated back to the previous separation step, e.g. segment, from each separation step to the separation device. In one embodiment, at least a fraction of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated continuously. In one embodiment, at least a fraction of the washing filtrate and / or soluble carbohydrate containing fraction is recirculated in each separation step or in each separation step. An amount of washing water can be reduced by means of recirculation.

In one embodiment, the washing filtrate is recirculated, preferably completely, to the lignocellulose material. In one embodiment, 80 - 100 w-% of the washing filtrate is recirculated to the lignocellulose material. In one embodiment, the washing filtrate contains washing water and carbohydrates such as galactose, glucose, mannose, arabinose, xylose, glucuronic acid and galacturonic acid. Further, the washing filtrate may contain soluble lignin.

In one embodiment, at least a portion of the soluble carbohydrate-containing fraction is recirculated to lignocellulose material. In one embodiment below 80 w-%, in one below 50 w-%, in one below 50 w-%, and in one below 20 w-%, of the soluble carbohydrate containing fraction of all liquid with soluble carbohydrates and oth- er compounds are recirculated to the lignocellulose material.

In one embodiment, the recirculation rate of the soluble carbohydrate containing fraction without the washing filtrate can be 0 to 95%, more preferably 60 to 90%, in one step process. When the washing filtrate is also used as a dilution water recirculation rate of the soluble carbohydrate containing fraction can be 0 to 90%, more preferably 35 to 80%, in one step process.

In one embodiment, at least a portion of the soluble carbohydrate-containing fraction is recirculated to lignocellulose material. In one embodiment, the washing filtrate is recirculated to lignocellulose material. In one embodiment, a mixture of the washing filtrate and the soluble carbohydrate containing fraction is recirculated to the lignocellulose material. In one embodiment, the washing filtrate and the soluble carbohydrate containing fraction are mixed to form a mixture, and the mixture is recirculated to the lignocellulose material.

Preferably, the feed concentration of the lignocellulose material is optimized by the recirculation composition.

In one embodiment, the sugar concentration of the soluble carbohydrate containing fraction is optimized. Preferably, the soluble carbohydrate containing fraction contains soluble C5 carbohydrates. Total carbohydrate content can be measured with HPLC after acid hydrolysis according to standard SCAN-CM 71:09. Monomeric carbohydrate content can be measured with HPLC from liquid fraction directly without acid hydrolysis. The soluble carbohydrate containing fraction may also contain C6 carbohydrates, preferably below 20 w-%. Preferably, the soluble carbohydrate-containing fraction can contain other monosaccharides, disaccharides, oligosaccharides, and / or polysaccharides. In one embodiment, the soluble carbohydrate containing fraction contains galactose, glucose, mannose, arabinose, xylose, glucuronic acid and galacturonic acid. In one embodiment, the soluble carbohydrate containing fraction comprises soluble C5 carbohydrates, such as Ο5Η10Ο5 or C5 (H2O) n, and other carbohydrates and some other compounds. In one embodiment, the soluble carbohydrate containing fraction contains more than 50 g / l, preferably more than 70 g / l, more preferably more than 100 g / l after the solid-liquid separation. In one embodiment, the soluble carbohydrate containing fraction is below 250 g / l, in one solution below 200 g / l, in one solution below 150 g / l after the solid-liquid separation. In one embodiment, the soluble carbohydrate containing fraction is between 15 to 280 g / l, preferably 30 to 200 g / l, more preferably 50 to 165 g / l after the solid-liquid separation. Preferably, the soluble carbohydrate containing fraction is in the form of a solution. In one embodiment, water soluble matter is between 20 to 425 g / l, preferably 45 to 303 g / l, more preferably 75 to 250 g / l after the solid-liquid separation. Water soluble matter can be determined by means of a method described later as the "gravimetric washing method".

Preferably, at least a portion of the soluble carbohydrate-containing fraction is supplied from the separation step. The soluble carbohydrate containing fraction can be supplied after any desired step of the separation step. In one embodiment, the soluble carbohydrate containing fraction is supplied after the first step of the separation step.

In one embodiment a soluble carbohydrate containing fraction (10) with a high concentration can be formed. The soluble carbohydrate containing fraction is formed from a lignocellulose material (3) which has been formed by treating a plant based raw material (1), whereby the soluble carbohydrate containing fraction has been formed by separating the soluble carbohydrate containing fraction (10) and / or a washing filtrate (12) from solid lignocellulose material (3) in one or more separation stage (4,6) and by recirculating at least a fraction of soluble carbohydrate containing fraction and / or washing filtrate to lignocellulose material for increasing concentration of soluble carbohydrate containing fraction. The soluble carbohydrate containing fraction may be used as a component in the manufacturing of the final product.

In one embodiment, a fraction of the soluble carbohydrate containing fraction (14) is separated from the lignocelluloses material (3) in connection with the pretreatment step (2,5) in which the lignocellulose material is formed and / or treated. The soluble carbohydrate containing fraction (14) may be separated by means of a similar separation method or device as used in the separation step (4,6) or by means of another suitable separation method or device.

In one embodiment, two soluble carbohydrate containing fractions (10,14) with high concentration can be formed with high soluble compound recovery. Two soluble carbohydrate containing fractions are formed from lignocellulose material (3) which is formed by treating plant based raw material (1) in two or more steps. The first soluble carbohydrate-containing fraction (14) is formed by separating a portion of the soluble compounds (2.5) and the second soluble carbohydrate-containing fraction (10) is formed by separating most of the soluble compounds after the last pretreatment step. Preferably, the second soluble carbohydrate containing fraction (10) is separated in the separation stage (4) so that the soluble carbohydrate containing fraction and / or the washing filtrate is separated from the solid lignocellulose material and at least part of the soluble carbohydrate containing fraction and / or washing filtrate is recirculated to lignocellulose material for increasing concentration of soluble carbohydrate containing fraction. The soluble carbohydrate containing fractions (14) and (10) may be combined or used separately as a component in the manufacturing of the final product. The combined or separate soluble carbohydrate containing fractions can be concentrated for further use.

In one embodiment, two soluble carbohydrate containing fractions (10,14) with high concentration can be formed with high soluble compound recovery. Two soluble carbohydrate containing fractions are formed from lignocellulose material (3) which is formed by treating plant based raw material (1) in two or more steps. The first soluble carbohydrate containing fraction (14) is formed so that the liquid to solid ratio (w / w) of the lignocellulose material is below 5: 1, preferably below 4: 1, and most preferably below 2: 1 before separating a part of the soluble compounds between the first and the last pretreatment steps (2,5). The second soluble carbohydrate containing fraction (10) is formed by separating most of the soluble compounds after the last pretreatment step. Preferably, the second soluble carbohydrate containing fraction (10) is separated in the separation stage (4) so that the soluble carbohydrate containing fraction and / or the washing filtrate is separated from the solid lignocellulose material and at least part of the soluble carbohydrate containing fraction and / or washing the filtrate is recirculated to the lignocellulose material for increasing the concentration of the soluble carbohydrate containing fraction. Fresh washing water is less than 4: 1 (liquid: solid (w / w)), preferably less than 3: 1, more preferably less than 2: 1, most preferably close to 1: 1. The efficiency of removing soluble carbohydrate containing fraction from solid to high and higher than 60%, preferably greater than 70%, more preferred than 80%, most preferred more than 90%. The soluble carbohydrate containing fractions (10 and (14) may be combined or used separately as a component in the manufacturing of the final product. The combined or separate soluble carbohydrate containing fractions can be concentrated for further use.

In one embodiment, a soluble carbohydrate containing fraction (10) with a high concentration can be formed with a high soluble compound recovery. The soluble carbohydrate containing fraction is formed from lignocellulose material (3) which is formed by treating plant based raw material (1) in one or more steps. The soluble carbohydrate containing fraction is formed by separating most of the soluble compounds after the last pretreatment step (2,5) so that the soluble carbohydrate containing fraction and / or the washing filtrate is separated from the solid lignocellulose material and at least a part of the soluble carbohydrate containing fraction and / or washing filtrate is recirculated to lignocellulose material for increasing concentration of soluble carbohydrate containing fraction. The soluble carbohydrate containing fraction may be used as a component in the manufacturing of the final product. The soluble carbohydrate containing fractions can be concentrated for further use.

In one embodiment, a soluble carbohydrate containing fraction (10) with a high concentration can be formed with a high soluble compound recovery. The soluble carbohydrate containing fraction is formed from lignocellulose material (3) which is formed by treating plant based raw material (1) in one or more steps. The soluble carbohydrate containing fraction is formed by separating most of the soluble compounds after the last pretreatment step (2,5) so that the soluble carbohydrate containing fraction and / or the washing filtrate is separated from the solid lignocellulose material and at least a part of the soluble carbohydrate containing fraction and / or washing filtrate is recirculated to lignocellulose material for increasing concentration of soluble carbohydrate containing fraction. Fresh washing water is less than 4: 1 (liquid: solid (w / w)), preferably less than 3: 1, more preferably less than 2: 1, most preferably close to 1: 1. The efficiency of removing the soluble carbohydrate containing fraction from the solid is higher than 70%, preferably greater than 80%, more preferably greater than 90%, most preferred more than 95%. The soluble carbohydrate containing fraction may be used as a component in the manufacturing of the final product. The soluble carbohydrate containing fractions can be concentrated for further use.

In one embodiment, the soluble carbohydrate containing fraction is recovered. In one embodiment, the soluble carbohydrate containing fraction is supplied to further processing. In one embodiment, the monomerization of the soluble carbohydrate containing fraction is made before further processing. In one embodiment, the soluble carbohydrate containing fraction is supplied to the fermentation process. In one embodiment, the soluble carbohydrate containing fraction is used as a source material in the fermentation. In one embodiment, the soluble carbohydrate containing fraction is supplied to a hydrolysis process. In one embodiment, the soluble carbohydrate containing fraction is used as a source material in hydrolysis such as by acid hydrolysis, Enzymatic hydrolysis or the like. In one embodiment, the soluble carbohydrate containing fraction is supplied to the Catalytic Treatment Process. In one embodiment, the soluble carbohydrate containing fraction is used as a source material in the Catalytic process. The soluble carbohydrate containing fraction may be supplied directly to the fermentation, hydrolysis, catalytic treatment process or other suitable process, or alternatively via a suitable treatment step, e.g. additional concentration step or purification step, to a fermentation, hydrolysis, catalytic treatment process or other suitable process.

In one process, at least a part of the washing filter is supplied to another process or process step. In one embodiment, the washing filtrate is used as a dilution water in the other process, e.g. in the pretreatment process. In one process, the washing filtrate is used as a washing water in the other process.

Solids (11) are supplied from the solid-liquid separation stage (4,6). In one embodiment, a solid fraction comprising solids is supplied from the solid-liquid separation stage. In one embodiment, the solid fraction consists of solids (11) is formed from lignocellulose material (3) which is formed by treating plant based raw material (1) so that the solid fraction is formed by separating a soluble carbohydrate containing fraction (10) ) and / or a washing filtrate (12) from solid lignocellulose material by means of at least one solid-liquid separation step (4,6) and by recirculating at least a portion of the soluble carbohydrate containing fraction and / or washing filtrate to the lignocellulose material (3), and the solids (11) have been recovered from the separation stage. In one embodiment, the solids comprise C6 carbohydrates such as (C6H12O6 or (C6 (H2O) n) / other solid carbohydrates and lignin, and some other compounds such as some residual soluble material. the form of a cake In one embodiment, the dry matter content of the cake is 40 -80% by weight, preferably 45 - 70% by weight, preferably preferably 50 - 60% by weight, after the solid-liquid separation step. one to one, dry matter content of the cake is 7 to 70% by weight, preferably 15 to 45% by weight, more preferably 25 to 35% by weight, after one solid-liquid separation step. soluble compounds below 15%, preferably below 6%, more preferably below 3% by weight, after one solid, liquid soluble matter is determined by a gravimetric washing method be done as follows: dry matter content (DM%) of raw ma terial, e.g. the solid and soluble fraction measured at 60 ° C, the amount of solids remaining after heating the sample at 60 ° C to the constant weight is measured and the dry matter content is calculated based on the wet and dry weights. For washing about 10 g of bone dry from the wet material under examination, weighed (exact weighed amount) and mixed with hot water (50 ° C) in a vessel so that the total amount is 200 g, the mixture is mixed for 20 s ( Bamix Mono Freehand Food Blender, 'C' Blade, Speed 1 (7000 rpm)), Blend is Soaked with Soaking Time 5 min, Bamix Mono Freehand Food Blender, C 'Blade, Speed 1 (7000 rpm) rpm)), mass of a dry filter paper measured, mixture mixed by means of Buchner (dia.125 mm) and filter paper, an inward relief valve is closed when the cake is Matt (dry) in whole, a the filtrate is taken and the blender and the vessel is washed with the filtrate and the filtrate is filtered again through the cake, the cake is washed three times with hot water, a 100 g, so that the suction effect is maintained all the time and washing water ( 100 g) is added when the cake is Matt (dry) in whole, the cake is weighed, the cake with the filter paper is dried in the foil dish, the dried cake (60 ° C) with the filter paper being weighed in the foil dish and the mass of the filter paper and foil dish being subtracted from the mass of the dried cake, the filter paper and foil dish, and then soluble matter free solid, i.e. water insoluble solids (WIS) of wet material under investigation, can be determined. Water insoluble solids, WIS%, can be calculated: WIS% = (weight of washed and dried material, e.g., cake) / (weight of wet slurry for washing, e.g., raw material). Water soluble matter, WS%, of dry matter can be calculated: WS% = (dry matter (DM%) of original slurry, e.g., raw material) - (water insoluble solids, WIS%). In one embodiment, with high soluble material content (25% to 50% of total dry matter soluble), the solid fraction contains soluble compounds below 15%, preferably below 9%, more preferably below 5% by weight, after the solid -liquid separation stage, measured by gravimetric washing method. In one embodiment, with lower soluble material content (below 25% of total dry matter soluble) of the raw material, the solid fraction contains soluble compounds below 9%, preferably below 6%, more preferably below 3% by weight, after the solid- liquid separation stage, measured by gravimetric washing method.

Particle size of solid particles can be defined, e.g. by an optical measurement device such as the Metso FS5, or by a laser diffraction method such as the Coulter LS230. In one embodiment, the particle size of the solid particles can be defined based on ISO 16065-N or TAPPI T271. Fiber lengths of solid particles can be defined based on ISO 16065-N when fibers are defined as material longer than 0.2 mm. Fiber length of solid particles can be defined based on TAPPI T271 when fiber length is 0.01 to 7.60 mm. In connection with Metso FS5, Lc means contour length, i.e.. centerline fiber length, which is the fiber length measured from the fibers center line from one end to the other. Length-Weighted Lc (l) means Length-Weighted fiber length which is the average fiber length measured from the fiber distribution Weighted according to the TAPPI T271 standards. Weighted Weighted Lc (w) means Weighted Weighted fiber length which is likewise average fiber length measured from a fiber distribution Weighted according to TAPPI T271 standards. Arithmetic Lc (n) means arithmetic mean which is calculated from the population distribution of fibers. In this result the average length is calculated from the length distribution. FI (1)% means length Weighted distribution% (width> 10 pm, length <0.2 mm). Fiber width is measured as integral value from the middle of the fiber to the account for tapered ends.

In one embodiment, length-weighted particle length Lc (l) is below [(0.4) x (corresponding unrefined sulphate pulp fiber length)], preferably below [(0.3) x (corresponding unrefined sulphate pulp fiber length)], more preferable below [(0.2) x (corresponding unrefined sulphate pulp fiber length)], now preferable below [(0.1) x (corresponding unrefined sulphate pulp fiber length)].

In one embodiment, fine particle width (fraction 0 - 0.2 mm) is below [(0.7) x (corresponding to unrefined sulphate pulp fiber length)], preferably below [(0.6) x (corresponding to unrefined sulphate pulp fiber length)], more preferable below [(0.5) x (corresponding unrefined sulphate pulp fiber length)], now preferable below [(0.4) x (corresponding unrefined sulphate pulp fiber length)].

In one embodiment, the solid fraction comprises fine solid particles which are fiber-like or indefinable particles with a longest dimension shorter than 0.2 mm measured with optical Metso FS5 (fraction FI (1) of length Weighted Lc (l) measurements and calculations). In one, the solid fraction of Hardwood consists of particles with the longest dimension shorter than 0.2 mm over 70% (FI (1)> 70%), preferably over 80%, more preferably over 90% and most preferably over 98% by weight, defined by Metso FS5. In one, the solid fraction of Softwood consists of particles with the longest dimension shorter than 0.2 mm over 50% (FI (1)> 50%), preferably over 60%, more preferably over 70% and most preferably over 80% by weight, defined by Metso FS5.

In one embodiment, the solid fraction comprises fine solid particles which are fiber-like or indefinable particles. The length weighted length Lc (l) of the solid fraction is measured based on the TAPPI T271 standard includes all the particles detected and filling the requirements of the measurement. TAPPI T271 defines fiber length of material to have longest dimension from 0.01 to 7.60 mm.

In one embodiment, the solid fraction comprises fine solid particles which are fiber-like or indefinable particles. The length Weighted length Lc (l) of the solid fraction is measured with Metso FS5. The Length Weighted Lc (l) -value is 40% or less of the corresponding length of the unrefined sulphate pulp fiber, preferably 30% or less, more preferably 20% or less, most preferably 10% or less. And the width of the fine particle fraction of length Weighted particles (Lc (1) fraction 0 - 0.2 mm) is 70% or less of the width of the corresponding sulphate pulp fiber, preferably 60% or less, more preferably 50% or less, the most preferably 40% or less.

In one embodiment, the solid fraction of Hardwood comprises fine solid particles which are fi- ber-like or indefinable particles. The length Weighted length Lc (l) of the solid fraction is measured with Metso FS5. The length Weighted Lc (1) fractions over 0.2 mm fiber length is 50% or less, preferably 35% or less, more preferably 20% or less, most preferably 5% or less.

In one embodiment, the solid fraction of Softwood comprises fine solid particles which are fiber-like or indefinable particles. The length Weighted length Lc (l) of the solid fraction is measured with Metso FS5. The length Weighted Lc (1) fractions over 0.2mm fiber length is 60% or less, preferably 45% or less, more preferably 30% or less, now preferably 15% or less.

In one embodiment, a solid fraction comprising solids (11) is supplied from the solid-liquid separation stage (4,6,). In one embodiment, the solid fraction is supplied after the latest solid-liquid separation step. In one embodiment, at least part of the solid fraction is supplied out between two separation steps or between two separation steps.

In one embodiment, the solid fraction is supplied to the hydrolysis which may be selected from the group consisting of acid hydrolysis, enzymatic hydrolysis, supercritical hydrolysis and / or subcritical hydrolysis and their combinations, or to the manufacture of a composite material or a combustion process or other suitable process or their combinations. The solid fraction may be supplied directly to the hydrolysis, manufacture of the composite material, combustion process or other suitable process step or an additional step, e.g. additional concentration step or purification step, to hydrolysis, manufacture of a composite material, combustion process or other suitable process.

The method according to the present invention provides a soluble carbohydrate containing fraction and a solid fraction with high concentration and with good quality. The solid fraction has a very high concentration of lignin and glucan and its hydrated products. Further, the solid fraction has very high purity. In the present invention water balance can be optimized. Then the soluble carbohydrate content can be increased in the soluble carbohydrate containing fraction. The present invention demonstrates improved sugar recovery. Further, the present invention minimizes waste water, and decreases post-treatment costs of the soluble carbohydrate-containing fraction. High concentration is achieved with low energy consumption.

The present invention provides an industrially applicable, simple and affordable way of making the soluble carbohydrate containing fraction with high concentration. The method according to the present invention is easy and simple to realize as a production process. The method according to the present invention is suitable for use in the manufacture of different sugar-based fractions and final products from different starting materials.

EXAMPLES

The invention is described in more detail with reference to accompanying drawings.

Example 1

In this example, the fraction containing the carbohydrate soluble is produced according to the process of Figure 1.

The lignocellulose material (3) is formed from plant-based raw material (1) by means of pretreatment (2). The lignocellulose material (3) is fed into a solid-liquid separation stage (4) comprises a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material (3) in the washing step of the pressure filtration. The washing filtrate (12) and the least fraction of the soluble carbohydrate containing fraction (10) are recirculated to the lignocellulose material before the pressure filtration device. A solid cake (11) containing e.g. solids, solid carbohydrates, lignin and some soluble sugar, Oligomer and polymer residual are removed from the pressure filtration device.

Example 2

In this example, the fraction containing the carbohydrate soluble is produced according to the process of Figure 2.

The lignocellulose material (3) is formed from plant-based raw material (1) by means of pretreatment (2). The lignocellulose material (3) is fed into a solid-liquid separation stage (4) comprises a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material (3) in the washing step of the pressure filtration. The washing filtrate (12) is recirculated to the lignocellulose material before the pressure filtration device. The soluble carbohydrate containing fraction (10) including C5 sugars is removed from the pressure filtration device. A solid cake (11) containing e.g. solids, solid carbohydrates, lignin and some soluble sugar, Oligomer and polymer residual are removed from the pressure filtration device.

Example 3

In this example, the fraction containing the carbohydrate soluble is produced according to the process of Figure 3.

The lignocellulose material (3) is formed from plant-based raw material (1) by means of pretreatment (2). The lignocellulose material (3) is fed into a solid-liquid separation stage (4) comprises a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material in the washing step of the pressure filtration. The washing filtrate (12) may be recirculated to the pre-treatment (2) of the lignocellulose material. Alternatively, the washing filtrate (12) is removed from the pressure filtration device and recirculated to another process. At least a fraction of the soluble carbohydrate containing fraction (10) is recirculated to the lignocellulose material before the pressure filtration device. A solid cake (11) containing e.g. solids, solid carbohydrates, lignin and some soluble sugar, Oligomer and polymer residual are removed from the pressure filtration device.

Example 4

In this example, the fraction containing the carbohydrate soluble is produced according to the process of Figure 4.

The lignocellulose material (3) is formed from plant-based raw material (1) by means of pretreatment (2). The lignocellulose material (3) is fed into a solid-liquid separation stage (4) comprises a filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material in the filtration. At least a fraction of the soluble carbohydrate containing fraction (10) is recirculated to the lignocellulose material before the filtration device. A solid cake (11) containing e.g. solids, solid carbohydrates, lignin and some soluble sugar, Oligomer and polymer residual are removed from the filtration device.

Example 5

In this example, a fraction containing the carbohydrate containing a soluble is produced according to a two-step process of Fig.5.

The lignocellulose material (3) is formed from plant based raw material (1) by means of pretreatment (2), e.g. by milling. The lignocellulose material (3) is fed into the first solid-liquid separation stage (4) comprising a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material (3) in the washing step of the pressure filtration. The washing filtrate (12) and at least part of the soluble carbohydrate containing fraction (10) are recirculated to the lignocellulose material before the first pressure filtration device. The fraction of soluble carbohydrate containing fraction (10) may be removed from the process before the second separation step.

In the second step, the lignocellulose material (3) is treated by means of a treatment stage (5), e.g. by physical, chemical or physic-chemical treatment such as by microwave or ultrasound treatment, or by steam explosion. The lignocellulose material is fed into a second solid-liquid separation step (6) comprising a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material in the washing step of the pressure filtration. The washing filtrate (12) and at least a portion of the soluble carbohydrate containing fraction (10) are recirculated to the lignocellulose material before the first and / or second pressure filtration device. At least a fraction of the soluble carbohydrate containing fraction (10) is removed from the process. A solid cake (11) containing e.g. solids, solid carbohydrates, lignin and some soluble sugar, Oligomer and polymer residual are removed from the pressure filtration device.

Example 6

In this example, the fraction containing the carbohydrate soluble is produced according to the two-step process of Fig.6.

The lignocellulose material (3) is formed from plant based raw material (1) by means of pretreatment (2), e.g. by milling. The lignocellulose material (3) is fed into the first solid-liquid separation stage (4) comprising a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material (3) in the washing step of the pressure filtration. The washing filtrate (12) and at least a portion of the soluble carbohydrate containing fraction (10) are recirculated to the lignocellulose material before the second separation device. The fraction of soluble carbohydrate containing fraction (10) may be removed from the process before the second separation step.

In the second step, the lignocellulose material (3) is treated by means of a treatment stage (5), e.g. by physical, chemical or physic-chemical treatment such as by microwave or ultrasound treatment, or by steam explosion. The lignocellulose material is fed into a second solid-liquid separation step (6) comprising a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material in the washing step of the pressure filtration. The washing filtrate (12) and at least a portion of the soluble carbohydrate containing fraction (10) are recirculated to the lignocellulose material before the second pressure filtration device. At least a fraction of the soluble carbohydrate containing fraction (10) is removed from the process. A solid cake (11) containing e.g. solids, solid carbohydrates, lignin and some soluble sugar, Oligomer and polymer residual are removed from the pressure filtration device.

Example 7

In this example, the fraction containing the carbohydrate soluble is produced according to the process of Fig.7.

The lignocellulose material (3) is formed from plant-based raw material (1) by means of the first pre-treatment (2), e.g. by hydrolysis. After the pre-treatment part of the soluble carbohydrates (14) is separated (13) in connection with the first pre-treatment step (2). The lignocellulose material (3) is fed into the second pre-treatment step (5) in which the lignocellulose material is treated, e.g. by steam explosion. After that the lignocellulose material (3) is fed into a solid-liquid separation step (4) comprising a pressure filtration device. A soluble carbohydrate containing fraction (10) containing C5 sugars is separated from the lignocellulose material by pumping and pressing step of pressure filtration. The washing filtrate (12) is separated from the lignocellulose material (3) in the washing step of the pressure filtration. The washing filtrate (12) and the least fraction of the soluble carbohydrate containing fraction (10) are recirculated to the lignocellulose material before the pressure filtration device. A solid cake (11) containing e.g. solids, solid carbohydrates, lignin and some soluble sugar, Oligomer and polymer residual are removed from the pressure filtration device. At least a fraction of the soluble carbohydrate containing fractions (10,14) is removed from the process.

Example 8

In this example a fraction of carbohydrate containing soluble is produced.

Birch wood chips were pretreated in one-step autohydrolysis and steam explosion process to dissolve hemicellulose. The formed pretreated lignocellulose material was mixed with hot water and stirred for a few hours. The solid-liquid separation was then done with Ou-totec Larox FP 0.3 two way pressure filter as described in Table 1. The filtration area was 0.27 m2. To simulate the increase in concentration, the soluble carbohydrate containing filtrate (10) was first used as a dilution water from the next round, and again after the second filtration, the soluble carbohydrate containing filtrate was used in the third dilution. Finally 5 filtration rounds were done. Filtration conditions are shown in Table 1.

Table 1

Total carbohydrate content was measured based on SCAN-CM 71 standard: acid hydrolysis and HPLC was used. As seen in figure 8, the carbohydrate content is increasing very well in a line with a simulated concentration curve.

The simulation of the example was done with an assumption of 15.7% dissolving carbohydrate content of the pretreated lignocellulose material, which was also measured value of the lignocellulose material in Example 8. As seen in Figure 9, the concentration of the

soluble carbohydrate containing filtrate coming out of the process will reach a level of 104 g / 1 in a continuous process.

Example 9

In this example a fraction of carbohydrate containing soluble is produced.

Birch wood chips were pretreated in one-step autohydrolysis and steam explosion process to dissolve hemicellulose. The formed lignocellulose material was mixed with hot water and stirred for a few hours. Then the solid-liquid separation was done with Outotec Larox FP 0.3 two way pressure filter as described in Table 1. The filtration area was 0.27 m2. Amount of washing water was 2: 1 (water: water insoluble solids).

To simulate the increase in concentration when all the washing filtrate (12) of the process and some soluble carbohydrate containing filtrate (10) of first pressing was calculated to use as dilution water of the next round, and again after the second filtration of the washing filtrate and some soluble carbohydrate containing filtrate of pressing was used in dilution of third filtration. In this case about 77% of the dilution liquid was soluble carbohydrate containing filtrate. The fraction containing the recirculated soluble carbohydrate was 70% of the total liquid with soluble compounds. Washing efficiency was assumed to be 90%. Finally more than 70 iteration rounds were done. The simulation of the example was done with an assumption of 15.7% of the dissolving carbohydrate content of the pretreated lignocellulose material, which was also a measured value of the lignocellulose material in example 8. As seen in Figure 10, the concentration of soluble carbohydrate containing the filtrate comes out of the process will reach a level of 102 g / 1 in a continuous process.

Example 10

In this example a liquid and solid fraction is produced.

Birch wood chips were pretreated in a two-step dilute acid steam explosion process to dissolve hemicellulose and to create a soluble carbohydrate containing fraction. Portion of this soluble carbohydrate containing fraction is removed before rapid pressure release of lignocellulose material in steam explosion. The lignocellulose material formed was mixed with hot water and stirred for a while. Then the solid-liquid separation was done with Outotec Larox PF 0.1 pressure filter as described in Table 2. The filtration area was 0.1 m2. Amount of washing water was 1: 1 (water: dry matter in the cake) and 3: 1. The results are shown in Table 3. Water soluble matter of dry matter is measured with gravimetric washing method.

Table 2

Table 3

Example 11

In this example a liquid and solid fraction is produced.

Birch wood chips were pretreated in a two-step dilute acid steam explosion process to dissolve hemi-cellulose. The lignocellulose material formed was mixed with hot water and stirred for a while. The solid-liquid separation was then done with a vacuum filtration filter as described in Table 4 (Vacuum filtration in laboratory). Filtration area was 0.1 m2. Amount of washing water varied from 0 to 8.6 (wa-ter: dry matter in cake).

Table 4

Example 12

In this example a concentrated liquid and a purified solid fraction are produced, based on example 10.

Birch wood chips were pretreated in a two-step dilute acid steam explosion process to dissolve hemicellulose. The lignocellulose material formed was mixed with hot water and stirred for a while. Then the solid-liquid separation was done with Outotec Larox PF 0.1 pressure filter as described in Table 2. The filtration area was 0.1 m2. Amount of washing water was 1: 1 (water: water insoluble solids in the cake) and 3: 1. The dry matter of the original pretreated biomass was 65%, the dry matter in the first filtration was 16%, and the water insoluble solid content was 13%. Water insoluble solid content was kept constant in filter press while dry matter of slurry was increased due to increased soluble material in slurry. The dry matter of the washed cake was about 50%. The composition of the solid fraction, which is further washed in the laboratory like in gravimetric washing method, is shown in Table 5. The solid fraction was washed with water in order to remove the residual soluble compounds, and after that the properties were determined.

To simulate the increase in concentration when all the washing filtrate (12) of the process and some soluble carbohydrate containing filtrate (10) of first pressing was calculated to use as dilution water of the next round, and again after the second filtration of the washing filtrate and some soluble carbohydrate containing filtrate of pressing was used in dilution of third filtration. In 1: 1 washing case about 83% of dilution liquid was soluble carbohydrate containing filtrate and in 3: 1 case 48% of dilution liquid was soluble carbohydrate containing filtrate. Washing efficiency was calculated to be 83% (1: 1) and 88% (3: 1). Finally more than 70 iteration rounds were done. Simulation of the example was done with measured soluble matter content of 18.4% of the pretreated lignocellulose material. The concentration of soluble matter containing the filtrate coming out of the process will reach a level of 135 g / 1 in a continuous process with 1: 1 washing and 99 g / 1 with 3: 1 washing.

Table 5

Example 13

In this example a soluble carbohydrate fraction and a solid fraction are produced.

Eucalyptus wood chips were pretreated in a one-step autohydrolysis and steam explosion process with two different process conditions to dissolve hemicel-lulose. The formed pretreated lignocellulose materials were washed with hot water in the laboratory to remove most of the water soluble compounds. These remaining, water soluble compound free solids were measured with two different particle size analyzers. The results of Metso FS5 and Coulter LS230 are presented in table 6 'two water insoluble solids of pretreated eucalyptus based lignocellulose materials'.

Table 6

The method according to the present invention is suitable in different embodiments to be used for producing the most different kinds of sugar based fractions from different raw materials.

The invention is not limited to the example referred to above; instead many variations are possible within the scope of the Inventive idea defined by the claims.

Claims (24)

1. A method for increasing concentration of a soluble carbohydrate containing fraction (10), in

5 which lignocellulose material (3) formed by treating plant based raw material (1) is conducted into a separation stage (4), wherein the method comprises at least one solid-liquid separation stage (4) for separating a soluble 10 carbohydrate containing fraction (10) and/or a washing filtrate (12) from lignocellulose material (3), and at least a part of the soluble carbohydrate containing fraction (10) and/or the washing fil15 trate (12) is recirculated to the lignocellulose material (3) for increasing concentration of the soluble carbohydrate containing fraction, and solids (11) and at least a part of the soluble carbohydrate containing fraction (10) are sup20 plied out from the separation stage.

2. The method according to claim 1, wherein the soluble carbohydrate containing fraction (10) and/or washing filtrate (12) are separated from lignocellulose material (3) by means of filtration, cen-

25 trifugal treatment or their combinations.

3. The method according to claim 1 or 2, wherein the solid-liquid separation stage (

4) comprises a filtration in which the filtration is carried out by pressure, underpressure or overpressure.

30 4. The method according to any one of claims 1 to 3, wherein the solid-liquid separation stage (4) comprises a washing in which a displacement washing of the lignocellulose material is carried out with small amount clean water in which ratio of washing water to

35 solid is below 6, preferably below 3 and more preferably below 1.5.

20185854 prh 12-10-2018

5. The method according to any one of claims 1 to 4, wherein the washing filtrate (12) is recirculated to the lignocellulose material (3).

6. The method according to any one of claims 1

5 to 5, wherein at least a part of the soluble carbohydrate containing fraction (10) is recirculated to lignocellulose material (3).

7. The method according to any one of claims 1 to 6, wherein a mixture of the washing filtrate (12)

10 and soluble carbohydrate containing fraction (10) is recirculated to the lignocellulose material (3).

8. The method according to any one of claims 1 to 7, wherein feed concentration of the lignocellulose material (3) is 2 - 60 % by weight, preferably 5-30

15 % by weight, more preferable 10 - 20 % by weight.

9. The method according to any one of claims 1 to 8, wherein the soluble carbohydrate concentrate of the soluble carbohydrate containing fraction (10) is between 15 to 280 g/1, preferably 30 to 200 g/1, more

20 preferable 50 to 165 g/1 after the solid-liquid separation .

10. The method according to any one of claims

1 to 9, wherein the solid-liquid separation stage (4) comprises more than one separation steps.

25

11. The method according to any one of claims

1 to 10, wherein the method comprises more than one solid-liguid separation stages (4,6).

12. The method according to any one of claims 1 to 11, wherein the plant based raw material (1) is 30 wood based material or a mixture comprising wood based material.

13. An apparatus for increasing concentration of a soluble carbohydrate containing fraction, in which the apparatus comprises a separation device (4) 35 into which lignocellulose material (3) formed by

20185854 prh 12-10-2018 treating plant based raw material (1) is conducted, wherein the apparatus comprises

- at least one solid-liquid separation device (4) for separating a soluble carbohydrate containing

5 fraction (10) and/or a washing filtrate (12) from lignocellulose material (3),

- at least one feeding device for feeding the lignocellulose material (3) into the separation device (4 ) ,

10 - at least one recirculation device for recirculating at least a part of the soluble carbohydrate containing fraction (10) and/or the washing filtrate (12) to the lignocellulose material (3) for increasing concentration of the soluble carbohy15 drate containing fraction, and

- means for supplying solids (11) and at least a part of the soluble carbohydrate containing fraction (10) out from the apparatus.

14. The apparatus according to claim 13, 20 wherein the apparatus comprises more than one solidliquid separation devices (4,6).

15. The apparatus according to claim 13 or 14, wherein the apparatus comprises at least one filtration device (4) and/or centrifugal device for separating

25 the soluble carbohydrate containing fraction (10) and/or washing filtrate (12) from lignocellulose material (3) .

16. The apparatus according to any one of claims 13 to 15, wherein the apparatus comprises at

30 least one pressure filtration device, vacuum filtration device, filtration device based on underpressure or filtration device based on overpressure for separating the soluble carbohydrate containing fraction (10) and/or washing filtrate (12) from lignocellulose 35 material (3).

20185854 prh 12-10-2018

17. A soluble carbohydrate containing fraction formed from lignocellulose material which is formed by treating plant based raw material, wherein the soluble carbohydrate containing fraction has

5 been formed by separating a soluble carbohydrate containing fraction (10) and/or a washing filtrate (12) from lignocellulose material and by recirculating at least a part of the soluble carbohydrate containing fraction and/or the washing 10 filtrate to the lignocellulose material for increasing concentration of the soluble carbohydrate containing fraction.

18. The soluble carbohydrate containing fraction according to claim 17, wherein the soluble carbo-

15 hydrate containing fraction comprises soluble C5 carbohydrates, such as Ο₅Η₁₀Ο₅ or Ο₅(Η₂Ο)_η, and other carbohydrates .

19. A solid fraction comprising solids formed from lignocellulose material which is formed by treating

20 plant based raw material, wherein

- the solid fraction has been formed by separating a soluble carbohydrate containing fraction (10) and/or a washing filtrate (12) from lignocellulose material by means of at least one solid-

25 liquid separation stage and by recirculating at least a part of the soluble carbohydrate containing fraction and/or the washing filtrate to the lignocellulose material, and

- solids (11) has been recovered from the separa-

30 tion stage.

20. The solid fraction according to claim 19, wherein the solid fraction comprises solid C6 carbohydrates, such as C₆H₁₂O₆ or C₆(H₂O)_nz· other solid carbohydrates and lignin.

35

21. The solid fraction according to claim 19 or 20, wherein the solid fraction contains soluble com pounds below 15 %, preferably below 6 %, more preferably below 3 % by weight, after the solid-liquid separation stage.

22. The solid fraction according to any one of

5 claims 19 to 21, wherein the solid fraction comprises fine solid particles with longest dimension shorter than 0.2 mm.

23. A Use of the soluble carbohydrate containing fraction formed according to any one of claims 1 to

10 12, wherein the soluble carbohydrate containing fraction is used as a source material in fermentation, hydrolysis, catalytic process or their combination.

24. A Use of the solid fraction comprising solids formed according to any one of claims 1 to 12,

15 wherein the solid fraction is used as a source material in hydrolysis, manufacture of a composite material, combustion process or their combination.