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Method of converting cellulose material to ethanol

Method of converting cellulose material to ethanol
IPC classes for russian patent Method of converting cellulose material to ethanol (RU 2432368):
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FIELD: chemistry.

SUBSTANCE: lignocellulose biomass is in form of maize stalks, chopped whole plants and pulp. The method involves infusion of lignocellulose biomass, followed by continuous hydrothermal preliminary treatment of the material at temperature 170-200°C. Infusion can be carried out in a liquid containing acetic acid. The lignocellulose biomass at the infusion step is saturated with organic acids formed at the next steps. Pre-treated material is then pressed to obtain a fibre fraction and a liquid fraction. The fibre structure of lignocellulose biomass is retained. Transfer of hemicellulose sugars from the lignocellulose biomass into the liquid fraction is not less than 60% of the initial content of lignocellulose biomass. Over 80% of lignin initially contained in the lignocellulose biomass is retained in the fibre fraction. The fibre fraction undergoes enzymatic softening and saccharification. Enzymatic softening of the fibre fraction takes place in a cylindrical drum fitted with a rotor with hoisting devices. As a result fermentation, lignin microparticles are suitable for co-combustion as solid fuel with coal dust. Part of the liquid fraction is used to obtain feed for ruminant animals.

EFFECT: method is energy saving and enables to obtain ethanol from lignocellulose biomass without adding acids, bases or other chemicals which must be extracted.

17 cl, 3 dwg

 

The technical field

The present invention relates to reliable methods for cost-effective and energy-efficient conversion of lignocellulosic biomass into ethanol and other products based on a continuous hydrothermal pretreatment and subsequent enzymatic hydrolysis, fermentation with obtaining ethanol and retrieval.

Background of the invention

Lignocellulosic biomass contains different amounts of cellulose, hemicellulose, lignin, and small amounts of protein, pectin, wax, potassium chloride and other inorganic compounds. Lignocellulosic biomass must be understood in its broadest sense, that is, it is, in addition to wood, residues of agricultural products, crops, used as an energy source, also contains different types of waste, both industrial and domestic. Cellulosic biomass is a huge underused resource, and in some cases creates a problem with waste disposal. However, hexose cellulose can be converted by the yeast into fuel ethanol, which has a growing demand. Pentose from hemicellulose still cannot be turned into ethanol on an industrial scale, but we have already developed several promising ethanologenic of microorganisms able to convert pentoses and hexose.

Until recently, the cost of cellulosic enzymes for the conversion of pretreated cellulosic feedstock in capable of fermentable sugar was too high.

This cost was greatly reduced due to successful research work carried out by companies Novozymes and Genencor, sponsored by the U.S. Department of energy.

However, requires a greater cost reduction in order to achieve cost-effective use of huge quantities of lignocellulosic raw materials.

Prior

In most ways prior raw materials are crushed or grinded into powder which is then mixed with water to obtain a liquid mass. This has several drawbacks:

- high energy consumption for grinding or crushing;

- large capital and operating costs for the grinding or crushing;

- requires large amounts of fluid to suspended particles in the curable pumping pump a lot that can be treated;

it is difficult again to remove the fluid mechanical spillway.

In addition, most of the methods of the prior art was tested only in laboratory scale, and they were not able to offer solutions for the transition to an industrial scale.

The conversion of cellulosic material in ethanolamine includes pre-processing of the pulp before the actual hydrolysis is able to fermentable sugar, to make the cellulose accessible to enzymes or chemical reagents. The total effect of elevated temperatures, residence time and chemical reagents is called the degree of seriousness of the process. This means that the same results can be achieved, for example, in a shorter time, if the temperature is higher. To make the cellulose accessible to cellulases, in most ways of pre-processing according to the prior art tend to dissolve and remove as much of the hemicellulose and lignin to form larger "pores" and to allow greater contact between cellulose and cellulase. The problem with the inhibitors formed during this type of pre-treatment, is solved in different ways, such as the introduction phase of detoxification or by the fastest possible removal of dissolved components.

In "The Alcohol Textbook", third edition, 1999, Chapter 9, J.S. Tolan conducts a review of the process of production of fuel ethanol from cellulosic biomass, implemented on a pilot installation of Iogen Corporation.

Tolan emphasizes that the process of pre-processing required to make the cellulose accessible to enzymes, and compares 3 operations:

- pre-processing-based solvent, where the organic will dissolve the al dissolves the lignin. However, lignin is not considered a significant barrier to pulp.

Alkaline pre-treatment, which does not form furfural, but reported the degradation of hemicelluloses.

For Iogen preferred pre-treatment with dilute acid, as it is soft for hemicellulose and gives a material with high surface area. In this way the lignin depolymerized, but not soluble, and low levels of acid eliminates the need to retrieve it. In the pre-treatment according Iogen fibrous structure of the raw material is destroyed, and it gets muddy texture and dark brown color.

Cellulase is produced mainly from the fungus Trichoderma in submerged liquid culture fermentation vats. Obtaining enzymes for ethanol plant has the advantages that the purification, concentration and storage can be omitted, and some hydrolysis of sugar can be used to obtain the enzyme.

According to preliminary processing by Iogen raw material is fed into the hydrolysis Chan as a liquid mass with a solids content of 15-20% or so, what can be processed. Mixing in a VAT weaker than is typically used in a fermentation VAT, but must be sufficient to keep the solid particles dispergirovannykh and PE is to Imamate material. Hydrolysis lasts 5-7 days. The viscosity decreases, and the particles lignocellulose become smaller. Will be converted to about 80-95% of cellulose, and the rest is inaccessible to enzymes, as it is covered by lignin.

In enzymatic conversion of cellulose into glucose problem is the inhibition products cellobiose and glucose. Often it was proposed to carry out the process of simultaneous saccharification and fermentation (SSF)to overcome the inhibition by products of glucose on β-glucosidase. However, the process of simultaneous saccharification and fermentation (SSF) has a non-optimal operating conditions, because the optimal temperature for the enzyme (50°C) and yeast (28°C) too far from each other, and the average temperature (37°C) carries the risk of contamination by germs. Another option is to obtain a β-glucosidase, adding additional costs due to additional fermentation process. In Iogen was selected to develop strains of Trichoderma to get more β-glucosidase.

Tolan describes a sharp decrease in the rate of transformation. After 24 hours it is less than 2% of the initial speed. The causes of this decline to the end of the incomprehensible.

Tolan lists several opportunities to improve the efficiency of enzymes:

more enzyme, less time, which, however, according to the authors of the present invention and Tolan Russ is arrivalsa as a disadvantage from an economic point of view.

- Recycling enzyme, which, however, requires further research.

- Continuous or batch feed system. This can provide a high concentration of cellulose in the whole time.

The best cellulase enzymes. Already there have been many studies, but this approach can be further developed with new technologies in molecular biology.

- New reactors. Have you done a lot of research, but in the evaluation of new reactors would be useful to have a better understanding of the effect of the enzymes.

- Best pre-treatment. This approach have been extensively studied, but still can be improved.

After hydrolysis of undissolved material, mainly lignin and residual pulp is separated from the liquid fraction at the plate and frame filter, washed 2-3 times with water to produce a high degree of extraction of sugar. The liquid fraction is pumped into fermentation vats, the solid fraction is subjected to spray-dried and burned to provide energy for the plant.

Tolan refers to the ongoing efforts to search for microorganisms that can ferment C5 sugars into ethanol, which at that time was not yet successful.

Report NREL 99-10600/18 "acid hydrolysis Reactors, sequencing batch system. Process design and cost estimation of important equipment is the process of converting biomass to ethanol" describes that serious problem is the corrosion of the equipment in acidic conditions and at high temperatures (high complexity). Periodic processes additional problem for equipment is that the temperature fluctuates between maximum working temperature and temperature loading.

Patent US 5503996 (Torget) describes prehydrolysis lignocellulose, in which the acid solution passes through the particle lignocellulose with the removal of soluble components as their education, which uses a flow-through system, where the fluid is moving relative to the solid lignocellulose. When prehydrolyzed hot biomass is separated into a solid fraction and the hydrolysate, the latter contains more than 90% hemicellulosic sugars, up to 25% cellulosic sugars and 20-50% of lignin Klason. The method of patent US 5503996 reaches such a degree of hydrolysis with a relatively small amount of added acid.

Patent US 6228177 (Torget) describes how hot rinse after pre-treatment to prevent re-deposition/condensation of lignin on cellulose. Hot washing is carried out at a temperature of about 140°C, which is considerably lower than the temperature of pre-treatment. Acid is added, or the pre-treatment, or during a hot flush. After the hot wash was measured Lucena cellulase digestibility. By combining the two processes described Torget, dissolve a substantial portion of the lignin (20-50%), most of which is washed with hemicellulose during hot washing. However, the wash water with a mixture hemicellulosic sugars and dissolved lignin is very difficult to turn into marketable products with economic value.

In Enerkem Technologies, Canada, developed the "FIRST" method of pre-processing, in which the raw material is impregnated with the acid followed by rapid steam processing. The advantage of this method is that it works with a high ratio of dry mass to liquid. The use of acid leads to various problems such as the formation of inhibitors and additional costs associated with extraction and processing of acid.

Patent US 6555350 B2 (Birgitte Ahring and Anne Belinda Thomsen) describes a method of pre-processing based on alkaline wet oxidation and steam explosion, where the fraction coming from the fermentation of obtaining ethanol, is treated by microorganisms to generate biogas and to reduce the content of inhibiting substances in the waste water to a level sufficient to return a more significant part in the process than the method without biogas.

The document US 2005/0069998 (Ballesteros) describes a method of pre-processing without the use of acid or other chemical reagents. E is from the method is based on steam explosion with subsequent separation into liquid and solid fractions. The solid fraction is subjected to simultaneous saccharification and fermentation (SSF)using heat-resistant strain of yeast to solve the problem of different optimal temperatures described Tolan. Describes that this method is not continuous and that the reactor is opened and closed manually. There are no instructions on how to zoom way up-scale industrial production.

Energy consumption for ethanol from grain is relatively high due to high demand in a pair for rectification, evaporation, heating etc. Complete consumption per kg of ethanol in modern processes reaches approximately at 3.25 mcal pair and 0.33 mcal, or 0,38 kW·h of electricity, which corresponds to approximately 50% higher calorific value of ethanol (7 mcal/kg). To meet these requirements, most ethanol plants are steam-generating equipment, but get electricity from the network. Some ethanol plants are combined heat and power (CHP), can produce all the steam and electricity required for the production process, but connected to the network, which allows them to receive and deliver moderate amounts of electricity.

Energy consumption for ethanol production from lignocellulosic raw materials such as grain straw and corn stalks, when applying the methods described by the prior art, much more in relation to as steam and electricity than for the production of starch-based/sugar. Therefore, the Association with combined heat and power (CHP) is of great interest.

Overview of the present status in this area is proposed in the article "Co-production of bio-ethanol, electricity and heat from biomass residue" J.H. Reith et al., presented at the 12th European conference and technology exhibition on biomass energy for energy, industry and climate protection, 2002.

This article compares the existing ethanol production based on starch and/sugariness crops with producing ethanol from cellulose.

The article offers thermal conversion of substantial amounts incapable of fermentation residues in combined-cycle power system of the integrated gasification of coal to support the needs for steam and electricity for the production process and receipt of surplus electricity for transmission in the network, which leads to a total efficiency of energy use 56-68%.

The article emphasizes that

there is no fermentation of a system suitable for the fermentation of pentoses from hemicellulose fractions

- you want at least a 10-fold increase in the efficiency cost of cellulase,

- the water flow rate 3-5 times higher than in obtaining ethanol from starch/sa is Ara, and

- should reduce capital costs by 30%to reach a value of ethanol competitive with the cost of ethanol from sugar/starch crops.

The report NREL "Study combining bioethanol production" concludes that there is great benefit in combining plant for the production of ethanol from cellulosic material with combined heat and power (CHP) and that this benefit will be even greater when the connection with the power plant that runs on fossil fuels. Some of the main benefits are:

- reduced capital costs,

- easy access to cheap pair and electricity

- equipment for combustion of residual lignin/cellulose

- reduced operating costs,

reliable fuel supply,

- access to the installed transmission networks and redistribution of bioelectricity.

The report emphasizes that the treatment of lignin and its co-combustion can lead to technical problems, because lignin is a material very different from coal.

Another problem that is underlined in the report is the difficulty of achieving economies of scale only remnants of lignocellulose as transportation over large distances as invalid for environmental and economic reasons. In the report it is proposed to develop with the person using a mixture of the residue lignocellulose and raw materials from starch/sugar or lignocellulosic energy crops, in order to obtain savings from increasing the scale of production.

Description of the invention

The first aspect of the present invention is an installation and method for the conversion of cellulosic material, such as shredded straw and corn stalks, chopped whole plant grain corn, sugar cane and household waste into ethanol and other products, and pulp material contains mainly cellulose, lignin, hemicellulose and ash. In the method according to the first aspect of the present invention the cellulosic material (also referred to as raw materials) are cleaned and subjected to continuous hydrothermal pre-treatment without the addition of acids or bases, or other chemical reagents, which must be removed, and receive the liquid and the fraction of fibers. Then how to apply liquid fraction, there are different alternatives, the fraction of fibers is subjected to enzymatic softening and saccharification. The method includes, in addition, fermentation of obtaining ethanol and selection of product. The method according to the first aspect of the present invention includes:

- implementation of hydrothermal pre-treatment, subjecting the cellulosic material to at least one operation of soaking and holding cellulosic material is at least one reactor high pressure that specifies an area of the high pressure reactor, working at high pressure; and cellulosic material is heated to a temperature from 170 to 230°C and subjected to cellulosic material is at least one operation of the centrifuge, forming a fraction of fibers and a liquid fraction;

- the choice of temperature and time of hydrothermal pre-treatment is carried out in a way that preserved the fibrous structure of the raw material and at least 80% of the lignin was kept in a fraction of fibers;

- download wrung fraction of fibers from areas of high pressure reactor in the below scheme closed zone, which is at a lower pressure than the high pressure zone of the reactor, with simultaneous collection of released steam without access for air;

- unloading of liquid fraction from the reactor high pressure in the second closed zone, which is at a lower pressure than the high pressure zone of the reactor, with simultaneous collection of released steam without access for air.

The first aspect of the invention relates also to an apparatus for conversion of cellulosic material to ethanol and other products, and pulp material contains at least cellulose, lignin, hemicellulose and ash, which includes a cleaning device for cleaning of pulp material, a device for hydrothermal pre-treatment, subjected to the cellulosic material continuous hydrothermal pre-treatment without the addition of acids or bases, or other chemical reagents that you want to extract, and this unit is suitable for receiving the liquid and the fraction of fibers, in addition, the installation includes a structure for carrying out enzymatic softening and saccharification fraction of fibers and the structure for fermentation with obtaining ethanol and extraction of the product, and the device hydrothermal pre-treatment designed to carry out the hydrothermal pre-treatment, subjecting the cellulosic material to at least one operation soaking; and where the installation includes:

at least one reactor high pressure, through which may be cellulosic material, and at least one reactor high pressure sets the high pressure zone of the reactor, which can operate at high pressure, and the reactor pressure vessels designed to heat the pulp material to a temperature of from 170 to 230°C, in addition, the reactor high pressure includes a pressing device for pressing the pulp of the material to thereby obtain a fraction of fibers and the liquid fraction, in accordance with the device for hydrothermal pre-treatment is performed so as to maintain such temperature and time on the hydrothermal pre-treatment to cornelluniversity structure of the raw material and at least 80% of the lignin was kept in a fraction of fibers;

the mechanism of unloading fraction of fibers for unloading wrung fraction of fibers from areas of high pressure reactor in the below scheme closed zone, which is at a lower pressure than the high pressure zone of the reactor, with simultaneous collection of generated steam without access for air;

the mechanism for discharging liquid for discharging liquid fraction from the reactor high pressure in the second closed zone, which is at a lower pressure than the high pressure zone of the reactor, with simultaneous collection of released steam without access for air.

In embodiments of the invention, the reactor high pressure may form or be in the device for hydrothermal pretreatment.

Method and installation according to the present invention can also provide an optional Association with the production of ethanol from sugar/starch raw material and, optionally, combining with combined heat and power (CHP).

The purpose of the preferred variants of the invention is to improve the economic and environmental efficiency of conversion of cellulosic material to ethanol. To achieve this, it is desirable that:

- gave way, in addition to ethanol, the residual organic product with low content of KCl, which could be turned into a pain the neck the amount of energy than is required for the process

the method could use raw materials of various types so that you can using the best raw materials

- all the components of the cellulosic material would be turned into marketable products,

the process was continuous,

all process steps can be carried out at high concentrations of dry matter,

- there was no waste of water

- the use of added water was very low,

- make the production of reliable and safe,

- no risk of contamination of air,

to the ethanol production was stable.

In preferred embodiments of the invention some of the measures to achieve these goals are:

- application of hydrothermal pre-treatment on the basis of soaking-pressed with a low degree of influence that allows you to save at least 80% of the lignin contained in the cellulosic material in the fraction of fibers in solid form.

- collection of steam released in the process of hydrothermal pre-treatment, and reuse in processes of evaporation,

- use of condensate from evaporation processes as added water,

- use of all neobrazovannyj liquids as raw materials or fertilizers

- the use of solid substances, incapable of fermentation, as the firm is on biofuels to generate more power, than is used in the process.

Instead of using a flow system in which the fluid has to move relative to the solid phase, the method according to the invention preferably uses a system of soaking-squeezing.

In this context, soak it assumes that there is enough liquid so that a substantial part of it can be removed by using the selected device is pressed. Pressing suggests that a significant portion of the liquid is again removed by mechanical means.

Operations soaking-pressing require, to preserve the fibrous structure of the material. Therefore, it is preferable that the method was carried out with a high content of relatively large particles.

When applying operations soaking-pressed:

- you can eliminate or at least reduce energy demand and expensive crushing and grinding,

- the ratio of water to dry weight of cellulosic material can be reduced to 6:1 or even lower,

- reliable contact between the solids and the liquid can be achieved at higher concentrations of dry solids in the reactor than in a flow system,

- the equipment is able to work with large objects, such as books and large chunks of unused food from waste, and to prepare them for the process of softening. Even nespos the service to the fermentation objects such as pieces of plastic, can undergo hydrothermal pre-treatment and sorted out after softening.

Unlike the most part of methods of the prior destruction of the maximum possible amount of hemicelluloses and lignin fraction of fibers during the pre-treatment is not a goal of the method according to the invention. Although Applicants do not wish to be bound by any particular theory, they believe that the lignin melts in the presence of water, and the hydrophobic lignin will form droplets, which otherdata at low temperatures and form microparticles without any or with very small effect protection of the pulp. When the hemicellulose and lignin does not need to be removed from fractions of fibers, pre-processing can be carried out at a lower degree of impact.

The low-impact, has the following advantages:

- you can not use acids and bases that you want to retrieve, which saves capital and operating expenses, as you can do without regeneration equipment, also significantly reduced problems with corrosion,

- you can save the fibrous structure of raw materials

decreases the formation of inhibitors,

dissolves very little lignin.

Further details the e describes some of the preferred options stages of implementation of the invention.

Cleaning of raw materials

Because cellulosic material often contains impurities such as stones, sand and other unwanted objects, it is advantageous to clean it up somewhat. In the case of some types of dry materials, such as straw, have problems with dust, since it leads to poor production conditions, the risk of fire and explosion dust. Wet campusuite will simultaneously clean pulp material from stones, sand and other heavy items, and wet pulp material that will solve problems with dust. If cellulosic material to crumble, it is advantageous to crumble him after he was soaked in compulabel, as most cellulosic materials easier to chop when they are wet. Wet compulsively can be combined with the pre-soaking explained later, so that the reactor pre-soaking acted as campusuite.

Hydrothermal pretreatment by soaking-wringer

- Hydrothermal pre-treatment is carried out as extraction with hot water, resulting in a fraction of fibres, containing the main part of the cellulose, more than 80% of the lignin present in the cellulosic material, and the liquid fraction, containing some of C5-sugars from hemicellulose, a large part is shown alkali chlorides, contained in the cellulosic material, and most of the inhibitors of fermentation (mainly acetic acid)obtained by hydrothermal pre-treatment.

- Cellulosic material is passed through at least one reactor high pressure that specifies an area of high pressure reactor operating at high pressure, and the cellulosic material is heated to a temperature from 170 to 230°C for the implementation of the hydrothermal pre-treatment. The temperature may range from 180 to 210°C, for example from 190 to 200°C.

- Unloading fraction of fibers from areas of high pressure reactor in the below scheme is a zone of high pressure, which is at a lower pressure than the high pressure zone of the reactor, with simultaneous collection of released steam without access for air. The preferred dry matter content is 20-60%, preferably 30-50%, and most preferably 35-45%.

- Unloading of liquid fraction from the reactor high pressure above the high pressure zone, which is at a lower pressure than the high pressure zone of the reactor, with simultaneous collection of released steam without access for air.

One the first stage of hydrothermal pre-treatment may include soaking at atmospheric pressure and temperatures of the x to 100°C, which may take place in containing acetic acid liquid fraction with subsequent stages. The purpose of soaking is to displace air from the raw material and to ensure saturation of the whole raw material liquid. Next goal is to use part of the energy of the liquid fraction to raise the temperature of the raw material. Other objectives of the stage soaking is to increase the dry matter content of the liquid fraction and soak raw organic acids formed in the later stages.

Before or during the transition to the next stage it is necessary to conduct an operation of pressing the cellulosic material. The objectives of the operation are pressed to increase the concentration of the solid phase, to avoid unnecessary heating of the liquid and transfer of dissolved material in the liquid fraction.

The next step might be handling high pressure at temperatures from 170°C to about 230°C, carried out, for example, as the process of ideal displacement with high solids content. High temperature is achieved by adding hot water or steam. If you add pairs, part of it will condense on cooler cellulosic material. Adding water or steam allows this technological stage to act as a second operation soaking.

In order to achieve the desired economic benefits, at least stage hydrothermal prior the nutrient processing, conducted at high pressure, preferably should be carried out at high concentrations of solid dry mass in the reactor. Thus, the reactor is preferably filled to 100%, and for bulky materials provided option is to seal. Often a cost-effective solution reactors are continuous with a high content of dry solids, based on the helical device, but in the case of 100%filling of the transport function of screw devices may not be enough. Therefore, embodiments of the reactor can include devices with two vzaimostsepljaemost screws or device with a single screw reciprocating axial movement. On the industrial scale, these reactors and screw devices will be so large that they can easily handle large objects.

Pre-processing based on the processing of water without the addition of acids, bases or other chemicals that you want to retrieve. This means that from raw materials in the liquid fraction (extract) is transferred less dry matter than in most other ways of pre-processing.

The transfer of lignin will usually be less than 20% of the original content in raw materials. A significant part of the hemicelluloses usually bude order to either hydrolyzed, but mostly oligomers and soluble polymers from which the liquid fraction will be moved only a small part.

What acid is not added, allows cellulosic material to retain the fibrous structure, which is desirable in order to carry out these operations of extraction, and this means low formation of fermentation inhibitors. In addition, small amounts of inhibitors (mainly acetic acid) will be concentrated in the liquid fraction from pre-treatment where, if necessary, with a low cost you can spend detoxification. Detoxification, if needed, for the method according to the invention preferably is carried out using NH3.

The concentration of solid dry mass when soaking will be 10-20%, and after wringing 30-40%, so approximately 2.5-3.5 kg of fluid per kg dry solid mass is added when the soaking and again removed during the spin cycle.

Each stage of soaking and pressing will move the dry weight of the solid in the liquid fraction.

The main purpose of hydrothermal pre-treatment according to the invention is to make the cellulose available for enzymatic hydrolysis/attack. In contrast, for example, from the way Torget special purpose is not the removal of hemicelluloses and lignin fraction of fibers, and the neutralization of their protection of the pulp. Although C is the registrants do not want to be bound to any specific theory, they believe that when the lignin is melted in the presence of water, the hydrophobic lignin will form droplets, which are dried at low temperatures to form microparticles without any or with only a small effect protection of the pulp. In terms of the melting of lignin during hydrothermal pretreatment hemicellulose will be either hydrolyzed to such an extent that it no longer protects the cellulose from the attack of enzymes. It is also believed that the melting conditions of lignin will fade the crystallinity of cellulose, which is beneficial for achieving effective enzymatic hydrolysis, however, the fibrous structure of the cellulose material will be maintained. To improve the allocation of molten lignin from the cellulose fibers, the raw material is subjected to the action of shear forces. They will wipe the lignin with cellulose and facilitate the formation of free hydrophobic droplets of lignin. Drops, apparently covered with hydrophilic compounds, resulting mainly from partially hydrolyzed hemicelluloses. It was unexpectedly found that the resulting microparticles lignin have a very small inhibitory effect or no inhibitory effect on the enzymatic hydrolysis and fermentation of obtaining ethanol, based on the yeast. The main advantage of this on the move, that:

- hydrothermal pre-treatment according to the invention can be carried out in less stringent conditions, which, as described earlier, reduces capital and operating expenses

- facilitated the separation of the pretreated cellulosic material at a fraction of fibers and the liquid fraction.

Shear forces can be applied by various means, such as conveyor device in the reactor, a device driven conveyor device, or by pressing at the loading and unloading of the reactor. Shear forces can also be directed through a steam explosion is used when unloading, the main effect of which is to break the cells and capillaries. Tool application shear forces can be applied independently or in combination of two or more funds.

An interesting result of the present invention is that the cut straw, held hydrothermal pre-treatment, is much more important than untreated straw because of better access to digestive enzymes.

One of the problems carried out on an industrial scale continuous pre-processing of bulk materials with a high concentration of long particles, such as straw of cereals or corn stalks, is moving so the first substrate in the reactor high pressure safe efficient and reliable way. It is advantageous to load raw material into the reactor portions using the boot device gateway type, such as a pump for the crushed material, described in WO 03/013714A1, and at any time at least one pneumatic shutter provides a tight seal between the reactor pressure vessels and vats for maceration. This pump is for the crushed material can remove the liquid from the soaked raw materials by extraction when loading into and unloading from the reactor and discharging can be combined with a steam explosion.

Also household waste, of which held up the diagram of the separation process were removed large or heavy components, but which still contain the remaining major parts such as cans, plastic bottles, pieces of plastic and wood, can be downloaded and uploaded the specified density for crushed material and processed in the reactor pre-treatment and softening. Nerazmeshchenie particles can be removed before or after fermentation. This is possible because all the preferred technological equipment according to the invention can take a relatively large particles.

In accordance with one embodiment of the present invention stage high pressure in the hydrothermal pre-treatment can lead wire is to be cleansed and purified in one or more embodiments of the conditions of temperature/pressure. The transfer of materials from one zone of high pressure to another will normally be carried out using a gateway system with a pressing device, such as a pump for the crushed particles described in WO 03/013714A1. Additional operations of extraction/soaking may be carried out within each zone of high pressure.

In accordance with one embodiment of the invention, when the hydrothermal pre-treatment is carried out at several variants of conditions temperature/pressure, temperature/pressure will increase with each stage. Because this process is counter-current with spin between each option conditions temperature/pressure, the amount of chemical exposure will decrease with increasing the degree of thermal effect, which is important to avoid problems of corrosion of the equipment. As during the hydrothermal pre-treatment acid forming, it also has the advantage that the pH in the fraction of fibers will be relatively close to neutral, as the liquid is added at the last stage, is not acidic. This means that the pH will be close to optimal for enzymatic softening, and require only minor adjustments. Removal of acid from the fraction of fibers is also advantageous when the substrate is a silo, as a high proportion of lactic acid bude is washed already in the preliminary soaking.

Pre-treated raw materials can be overcome when it is still in a high temperature environment with lignin in the form of droplets, or it can be overcome after it is unloaded from the reactor hydrothermal pre-treatment with lignin in the form of solid particles.

One advantage of the wringer before unloading of raw is that you can get a higher dry matter content in the fraction of fibers. Another advantage of pressed under high pressure and temperature is that the shear forces generated during the spin cycle, will provide improved release drops of lignin and splitting particles lignocellulose. The advantage of pressing at temperatures below 100°C is that lower costs, and that more lignin remains in the fraction of fibers.

The pressure relief as solid and liquid fractions can be carried out in closed systems without access of air to collect the emitted pairs and use thermal energy of steam in order to concentrate condensate as process water.

Unloading fraction of fibers can also be made through the pressing device, for example, by a screw press, as high pressure will fill the trough material, so that leakage is not allowed. This type of discharge should preferably PR is to live with the first phase, where pneumatic shutter between the reactor high pressure and below a closed compartment with the lower pressure is provided by a screw press, a conductive operation of the spin at the exit of the reactor high pressure, and the resulting liquid is drawn up the scheme, and the resulting solid phase is a fraction of fibers, below. The pressure in the specified closed compartment is preferably 2-6 bar. In the second phase, the fraction of fibers is directed on to the second closed compartment with a pressure of 1 bar or below the second screw press for pneumatic shutter between these two departments. Process water at a temperature lower than the temperature of the fraction of fibers is introduced into the second screw press at a first end of the screw, reducing the temperature of the fraction of fibres up to 100°C or below.

In order to obtain a sufficient enzymatic softening, it is desirable that as many enzymes were located on the surfaces of the available cellulose fibers contained in the particles pre-treated fraction of fibers. To achieve this, relatively warm wrung fraction of fibers are mixed with a relatively cold enzyme drug that can be absorbed in the cavity of the particles. Couples captured in the cavity, condenses, cools when the I enzyme preparation, and creates a vacuum, pulling the enzyme preparation in the cavity. Selecting the concentration of the enzymes in the product, you can put the desired number of enzymes on the inner and outer surfaces of the particles adhering to the cellulose fibers. Due to such adherence of the dry matter content in the filled enzymes fraction of fibers can be increased by pressing, at the same time preventing removal of enzymes to an unacceptable level.

Adjusting the temperature and pH of the enzyme preparation before mixing with the warmer pre-treated TF, it is possible to improve the conditions of tender.

According to Tolan, enzymes for hydrolysis of cellulose should typically contain three types of enzymes: endoglucanase, cellobiohydrolase and beta-glucosidase. The first two hydrolyzing a polymer cellulose to soluble dimeric cellobiose, which is then hydrolyzed to glucose by the enzyme of the third type. Inhibition by the product of cellobiose and glucose can be prevented or reduced by increasing concentrations of beta-glucosidase and use separate hydrolysis and fermentation. Another solution is to use a process of simultaneous saccharification and fermentation (SSF), and cellobiose and glucose into ethanol by fermentation of the organism. One way of implementing this is subramania based on the successful establishment of thermophilic ethanologenic microorganisms, having the ability to ferment and C5-and C6-sugars, and a compatible enzyme systems with high activity hemicellulase and cellulase at temperatures around 60°C and at a pH of about 6. Of particular interest to the present invention are thermophily with the ability to ferment not only monomers but also small oligomers, such as cellobiose, maltose and raffinose, which, together with a compatible enzyme the system will create a process of simultaneous saccharification and fermentation (SSF) for the conversion of pretreated according to the invention of biomass to ethanol. Alternatively, the method according to the invention can use the approach in which is introduced a separate stage softening, which gives optimal conditions for the enzyme activity, followed by the process of simultaneous saccharification and fermentation (SSF) with softened a fraction as the substrate and with the optimum conditions for fermentation of the organism, but with suboptimal conditions for enzymes.

During softening, catalyzed, for example, cellulases Tricoderma at a pH of about 5 and a temperature of about 50°C, endoglucanase can provide basic depolymerization, as the activity of cellobiohydrolase quickly inhibited accumulated cellobiose, and the activity of beta-glucosidase is inhibited accumulated glitch is zoé.

Softening may be carried out on the basis of two principles: liquid - or solid-phase softening.

For solid-phase softening filled with enzyme fraction of fibers is transferred to a mixer, which contains no free liquid in the input area.

For solid-phase softening in the industrial scale microscopic traffic enzymes from attack to attack, the pulp may not always provided with the usual stirring, so as to overcome the friction between particles requires large power consumption. Instead, technology can be applied, used in industrial composting, such as drums for composting, where the fraction of fibers filled with enzymes, undergoes a series of UPS and downs during transfer through a cylindrical drum which rotates or is stationary and is equipped with a rotor with lifting devices. After several hours, the resulting liquid will allow you to finish the process as a liquid softening.

Liquid-phase softening of the incoming particle fraction of fibers filled with enzyme, immersed in a viscous fluid the softened material. Even if the mixture viscosity, the mixing can be accomplished using various known mixing devices.

Some advantages of softening of the liquid state are

the dry matter content in the reactor may be high,

- transfer of appropriate efforts to ensure the movement of enzymes from attack to attack on cellulose fibers is facilitated by fluid

- possible return softened faction with enzymes in the input zone, which will create good conditions for active enzymes, so they can harass and attack the fresh pulp fibers.

The liquid-phase reactor softening according to the present invention may have the elongated cylindrical container with an inlet for full enzyme fraction of fibers in the upper part of one end of the container and the outlet for softened fraction (LfF) in the lower part of the other end of the container.

At the entrance perforated piston device can move the particle fraction of the fibers to exit completely immersed in the softened a fraction. At the output of the sieve device can separate the residual particulates consisting primarily of cellulose and lignin, softened fraction, consisting mainly of mud softened polysaccharides and suspended particulate lignin. When passing through the reactor structure of most particles lignocellulose will gradually disappear, and residual particulates can be sorted, split and return to the reactor inlet. Alternatively, the residual m is crocetti can be added in solid biofuel product.

And solid-phase and liquid-phase softening insensitive to large objects.

Microparticles of lignin can be removed or after the individual process of softening, or after the fermentation process known means, such as vacuum filtration or filtration under pressure, getting the filter residue with a high dry matter content, thanks to that achieved low costs for drying. This product usually has a low content of KCl and therefore can be burned in power plants with high electricity output. The filtrate can be injected into the supply tank, where the temperature, pH and nutrient content can be adjusted to optimize the conditions of the subsequent process of simultaneous saccharification and fermentation (SSF). If the process of simultaneous saccharification and fermentation (SSF) is based on the yeast, the temperature should be lowered to about 35°C and pH 5 can be saved.

If the process of simultaneous saccharification and fermentation (SSF) is based on thermophilic microorganisms, fermentation C6 and C5, such as thermopile company TMO Biotec, the temperature may be increased to about 60°C and pH to about 6.

This process of simultaneous saccharification and fermentation (SSF) can be conducted as a batch or continuous process, depending on the equipment, to the which is in itself known, as described in "The alcohol textbook" 3rd Edition 1999 Nottingham University Press.

Removing the ethanol can be carried out by ordinary rectification method.

The preferred technology of extraction of the present invention is a method of distillation, such as vacuum distillation, gas cleaning, or evaporation, by sputtering, in which the temperature of the fermentation mixture will remain close to the temperature of the fermentation when the removal of ethanol. Thereby limited by thermal inaktivirovanie enzymes and fermenting organisms, thus, enzymes and fermenting organisms may be returned into the cycle that gives further reducing costs.

Microparticles of lignin can be softened in fractions during fermentation, as microparticles macromolecular lignin do not have any or very little inhibitory effect. Simultaneous fermentation of obtaining ethanol and the extract is interesting cost alternative for the method according to the invention, where the ethanol is removed before the inhibition will begin to slow down fermentation.

The use of liquid fraction with hydrothermal pre-treatment depends on many factors, for example, from United whether this process with the process of ethanol production from raw sugar-based/Brahma is a, and whether competing organisms for the fermentation of C5. The preferred option of the invention is to neutralize contained acetic acid with NH3and combine it with filtered Barda with the conversion fraction of fibers, and the concentration of the mixture and use the syrup in feed for ruminant animals, ruminants can easily digest C5-sugars. This option has the advantage that N, P, K and other plant nutrients can be returned to the fields. If you develop a suitable microorganisms for the conversion of C5 sugars into ethanol, the mixture can be used as raw material for fermentation. It can also be used as raw material for production of single-cell protein, lactic acid and enzymes.

The Association of ethanol production from lignocellulosic raw materials with the production of ethanol from raw starch-based/sugar is advantageous variant of the method according to the invention, as it may result in a significant reduction in both capital and operating costs, especially in cases when it is difficult to recruit a sufficient number of lignocellulosic raw materials in order to obtain approximately 100,000 tons/year or more of fuel ethanol that is required to obtain economic benefits from increased scale of production. Furthermore, cost reduction can be achieved wealth is giving using at least a part or fraction liquid fraction from pre-treatment to replace the water or part thereof, necessary mash starch/sugar raw materials with high content of dry matter. This is possible if the liquid fraction obtained in accordance with the method according to the invention has a low content of inhibitors or does not contain inhibitors that normally takes place. A significant portion of the hemicellulose dissolved in the liquid fraction will be oligomeric, and therefore it is possible to separate the liquid fraction into two fractions by ultrafiltration. One fraction contains mainly pentose oligomers and has a high content of dry matter, while the other fraction (permeate) with low content of dry matter contains mostly alkaline chlorides and small organic molecules. This fraction is particularly suitable for replacement of added water in the mashing process grain. The oligomeric fraction pentoses can be used as raw material for fermentation in ethanol production, when you have the appropriate microorganisms fermenting C5-sugars. In addition, this fraction can be concentrated further and sold as raw material for ruminants. Microorganisms in ruminants can convert the pentose oligomers in short-chain fatty acids.

When raw materials are based on sugars/starch gives lignocellulosic residue (for example, grain corn, sugar cane), the remainder can be used as ligno cellulose raw materials.

Association with the production of ethanol from sugar/starch raw materials also opens the possibility for the supply of the source material from the world market, ensuring a more reliable supply of raw materials. It also opens the possibility to use as raw materials grain as a whole, which can significantly reduce the costs associated with harvesting, storage and transportation.

Another predominant variant of the method according to the invention is to combine the production of ethanol with existing Central power plants and to benefit from the use of a portion of low thermal energy, which would otherwise be discarded waste (sent to the installation of a condensing). A further reduction in cost is obtained from the lower capital costs due to the use of the power plant infrastructure. If the remains (mainly lignin) burned at the power plant, it is possible to achieve further economic improvement. Preferred embodiments of the method according to the invention give combustible residues of microparticles with low content of KCl that is well suited for co-firing with pulverized coal CHP with high electricity output, which means the value of balances by approximately 30% compared to the value achieved when the remains are burned at low thermal power plants designed DL who meet the energy needs of plants for biomass processing.

Example: conversion of wheat straw

The method of transformation according to the present invention was tested on sliced wheat straw on pilot equipment including wet cleaning and cutting of straw, pre-soaking and pre-processing high pressure reactor with two sections, with the first pump to the crushed material to download soaked raw materials in the first section, a second pump for the crushed material to transfer the raw material to the second section and a third pump for the crushed material to unload fraction of fibers of the second section. Pumps for the crushed material, used on the pilot plant described in WO 03/013714A1. This means that there may be three operations soaking-pressed using the pressing process pumps for the crushed material. In addition, it was tested stage of leaching at atmospheric pressure, at which the fraction of fibers after soaking was pressed by a screw press to a dry matter content of about 40%.

Evaluation of the effect of different pre-processing was based on data from experiments on the following below the softening, fermentation with obtaining ethanol and distilled pretreated straw.

The results of the conversion of pretreated straw following.

Composition per 1000 kg of wheat straw:

Moisture 140 kg
Cellulose 350 kg
Hemicellulose 250 kg
Lignin 150 kg
Ash 50 kg
More 60 kg

Process conditions:

Pre-soak: 80°C, 15 min

The reactor high pressure:

1st section: 180°C, 10 min

2nd section: 195°C, 3 min

3 operations soaking/spin

The ratio of water:straw = 5:1

Output:

Bioethanol 150 kg
Solid biofuels (90% suhm) (lignin and residual carbohydrates) 250 kg
C5 molasses (70% suhm)
Hemicellulose sugar, acetate and other
450 kg

In these technological conditions in C5-molasses contained a maximum of 4% (by dry weight) of lignin or products resulting from lignin, which corresponds to the content of lignin in the straw 12.6 kg, or 8.4%. This means that to 91.6% of the content of lignin in the straw kept varacchi fibers.

Similar results can be obtained in terms of process, when the first section of the reactor pressure vessels operated at 180°C for 17 min, and the second section is bypassed.

Experiments with wheat straw demonstrate that embodiments of the method according to the invention can provide a high degree of conversion of the cellulose content of the straw into ethanol, leaving about 90% of the lignin in the form of suspended solids that can be removed by known means.

Technological conditions according to the invention (temperature and time of stay) may be adjusted for cost-optimal for each commodity.

End of the example.

It should be understood that all the above in connection with the invention of distinctive features and achievements of the first aspect of the invention, and implementation options discussed below are applicable to the second aspect of the invention and/or option for its implementation.

The second aspect of the present invention are installation and method for the conversion of cellulosic material (CM) in ethanol and other products, and pulp material preferably contains cellulose and lignin, hemicellulose, and alkali chlorides, and possibly sugar. The method according to the second aspect of the present invention includes a continuous hydrothermal preparation is th processing (HTP) without adding acid, bases, or other chemical reagents that you want to extract, and subsequent enzymatic hydrolysis (EH), fermentation of obtaining ethanol and extraction. The method includes the steps:

- determination of the amount of elongated particles of cellulosic material (CM), such as straw and stalks by cutting and/or cutting before subjecting the cellulosic material (CM) hydrothermal pre-treatment (HTP). In the preferred distribution of particle sizes less than 5% of the particles have a length of more than about 20 cm, and less than 20% of the particles have a length of from about 10 to about 20 cm Cellulosic material (CM), including pieces of wood, preferably made sizes with standard chips.

- Preservation of the established size of the particles, i.e. the preservation of the structure of the particles during the hydrothermal pre-treatment and at the initial stage of enzymatic hydrolysis (EH).

- Implementation of hydrothermal pre-treatment such as extraction with hot water, thereby obtaining a solid fraction (TF), containing more than 80% of the lignin present in the cellulosic material (CM), and the liquid fraction (state) with the preferred content hemicellulosic sugars less than 80% of the original content in the CM, more preferably less than 70% of the initial content in the CM, even more preferably less than 60% of the TRANS is original content in the CM, containing most of these alkaline chlorides present in the cellulosic material (CM), and most of the inhibitors of fermentation, obtained by hydrothermal pre-treatment (HTP).

- Conducting cellulosic material (CM) through at least one reactor high pressure that specifies an area of high pressure reactor operating at high pressure, and the cellulosic material is heated to a temperature from 170 to 230°C for the implementation of the hydrothermal pre-treatment. The temperature may range from 180 to 210°C, for example from 190 to 200°C.

- Unloading particulate fraction (TF) of the zone of high pressure in the first reactor, below the scheme, the zone of high pressure, which is at a lower pressure than the high pressure zone of the reactor, preferably with simultaneous collection of released steam without access for air. The preferred dry matter content is 20-60%, preferably 30-50%, and most preferably 35-45%.

- Unloading of liquid fraction (state) from the reactor high pressure in the second zone of high pressure, which is at a lower pressure than the high pressure zone of the reactor, preferably with simultaneous collection of released steam without access for air.

The second aspect of the invention relates also to install the La transformation of cellulosic material (CM) in ethanol and other products, moreover, the cellulosic material preferably contains cellulose and lignin, hemicellulose and alkaline chlorides, and, optionally, sugar, and installing a continuous hydrothermal pre-treatment (HTP) without the addition of acids or bases and subsequent enzymatic hydrolysis (EH), fermentation of obtaining ethanol and extraction, where the installation includes:

a device for cutting or felling to determine the size of elongated particles of cellulosic material (CM), such as straw and stalks, before subjecting the cellulosic material (CM) hydrothermal pre-treatment (HTP);

device hydrothermal pre-treatment for the implementation of the hydrothermal pre-treatment such as extraction with hot water, and the device hydrothermal pre-treatment is able to maintain the prescribed particle size within the hydrothermal pre-treatment and to give a solid fraction (TF), containing more than 80% of the lignin present in the cellulosic material (CM), and the liquid fraction (state), containing the major part of these alkaline chlorides present in the cellulosic material (CM), and a large part of fermentation inhibitors formed during the hydrothermal pre-treatment (HTP);

at least one reactor in the high pressure specifies the zone of high pressure reactor operating at high pressure, and the cellulosic material is heated to a temperature from 170 to 230°C for the implementation of the hydrothermal pre-treatment;

- unloading mechanism for unloading the solid fraction (TF) of the zone of high pressure in the first reactor, below the scheme, the zone of high pressure, which is at a lower pressure than the high pressure zone of the reactor, and a discharge mechanism is preferably arranged to allow discharge to the collection of released steam without access for air and for discharging the liquid fraction (state) from the reactor high pressure in the second zone of high pressure, which is at a lower pressure than the high pressure zone of the reactor, preferably with simultaneous collection of released steam without access for air.

In variants of the implementation according to the first and second aspects of the invention, the second high pressure zone may be an upper high pressure zone, such as zone above the zone of high pressure reactor. It can be positioned lower relative to other areas, such as below the cutting or felling for regulating the size of elongated particles of cellulosic material and/or below the equipment for carrying out the hydrothermal pre-processing is I.

Preferred embodiments of the method and installation in accordance with the second aspect of the present invention include the determination of the amount of particles, the hydrothermal pre-treatment with the separation of the liquid and solid fraction, various operations for application of the liquid fraction, the enzymatic softening and solids saccharification, fermentation, and extraction of ethanol, optionally, combining with the production of ethanol from raw materials on the basis of sugar/starch and optional Association with combined heat and power (CHP).

One result of implementation variants of the present invention is to increase savings in the conversion of lignocellulosic materials into ethanol. Using the way in which the structure of the particles is maintained as long until you disappear on stage enzymatic softening (EL), and pre-treatment is carried out without addition of chemical reagents that you want to retrieve, you can perform a number of independent innovation to reduce costs and get fuel ethanol from lignocellulose value close to or cheaper than ethanol produced from raw materials based on starch/sugar.

The Association of ethanol production from lignocellulosic raw materials with the production of ethanol from raw starch-based/sugar is advantageous variant of the method according to image ateneu, as this can give a significant reduction in both capital and operating costs, especially in cases when it is difficult to recruit enough lignocellulosic raw material in order to obtain approximately 100,000 tons/year or more of fuel ethanol that is required to obtain economic benefits from increased scale of production. In addition, the cost reduction can be achieved by using at least a part or fraction liquid fraction (state) from pre-treatment to replace the water or part thereof, required for mashing starch/sugar raw materials with high content of dry matter. This is possible if the liquid fraction obtained in accordance with the method according to the invention has a low content of inhibitors or does not contain inhibitors that normally takes place. A significant portion of the hemicellulose dissolved in the liquid fraction (state), will be oligomeric, and, consequently, it is possible to separate the liquid fraction (state) into two fractions by ultrafiltration. One fraction contains mainly oligomeric pentose and has a high content of dry matter, while the other fraction (permeate) with low content of dry matter contains mostly alkaline chlorides and small organic molecules. This fraction is particularly suitable for replacement of water in the process of grouting grain (optional re the coy or chipping). During the pre-treatment pH of the liquid fraction (state) usually drops to about 3.5, preferably is adjusted to the optimum for yeast values with NH3. Fraction pentoses can be used as a fermentation feedstock for ethanol production, when there are relevant microorganisms fermenting C5-sugars. In addition, it can further thickening and sold as feed for ruminants. Microorganisms in ruminants can convert the pentose oligomers in short-chain fatty acids.

When the sugar/starch raw material gives lignocellulosic residue (for example, grain corn, sugar cane), the remainder can be directly used as lignocellulosic raw materials.

Association with the production of ethanol from sugar/starch raw materials also opens up the possibility of supply of the source material from the world market, ensuring a more reliable supply of raw materials. It also opens the possibility to use as raw material plants of cereals as a whole, which can significantly reduce the costs associated with harvesting, storage and transportation.

Another preferred alternative of the method according to the invention is to combine the production of ethanol from existing power plants and to benefit from the use of parts of low Teplov the th energy which would otherwise be discarded waste (sent to the installation of a condensing). A further reduction in cost is obtained from the lower capital costs due to the use of the power plant infrastructure. If the remains (mainly lignin) burned at the power plant, it is possible to achieve further economic improvement. Preferred embodiments of the method according to the second aspect of the invention give combustible residues of microparticles with low content of KCl that is well suited for co-firing with pulverized coal CHP with high electricity output, which means the value of balances by approximately 30% compared to the value achieved when the remains are burned at low thermal power plants designed to meet the energy needs of the installation for biomass processing.

Refining lignocellulosic feedstock prior to pretreatment is one of the most energy-consuming process stages used for the conversion of cellulosic material (CM) in ethanol. In most ways prior to obtain small particles with large surface area are used hammer crushers, but the effect of lignin as a strong thermoplastic adhesive forces at low temperatures to make very high mechanical effort to achieve the desired particle size.

In preferred embodiments, the implementation of this method of conversion crushing pre-processing generally does not apply, on the contrary, the structure of the particles is maintained during the entire pre-treatment in order to benefit from the huge surface area, given by the cavities of the cells and capillaries vegetable particles, to create a good reaction conditions for the hydrothermal pre-treatment (HTP) for the next stage of the tender. At high temperature hydrothermal pre-treatment (HTP) lignin is converted into a liquid, losing its quality as an adhesive, this means that it requires only a very weak mechanical force to open the cavity cells and to facilitate the access of cellulose enzymes to the inner surfaces of the particles.

Thus, the grinding can be replaced by the process of harvesting, receiving particles, most of which has a length of less than about 10 cm, and the smaller part has a length of about 20 cm and about 30 cm

Advantageous effect of the device and method according to the present invention is that the cut straw, held hydrothermal pre-treatment (HTP)can have the energy content for ruminants, more than twice the energy content of untreated straw, through improved access to food is artelinic enzymes.

In the case of some types of dry materials, such as straw, the problem is dust, because it leads to poor production conditions, the risk of fire and dust explosions. These problems can be solved by hydration of raw materials, which will also facilitate cutting and to reduce the specific energy consumption to a low level, for which the straw is only about 25% of the cost when using a hammer mill. For straw and similar materials will often be advantageous to remove stones and other impurities and to hold wetting in wet cannotdelete.

Felling of bulky raw materials, such as straw, can be facilitated by the seal of the raw material before it enters that zone logging.

For forest raw materials, the cutting device may include or be replaced by a device for receiving chips.

For materials with small particles, such as citrus, potatoes and sugar beet chips, crushed grain and sawdust, are not required to reduce the particle size may instead be advantageous to mix it with more fibrous raw materials.

For setting the size of the particles should hydrothermal pre-treatment (HTP). The purpose of hydrothermal pre-treatment (HTP) is to make the cellulose available for enzymatic hydrolysis/attack.

Pre-processing based on EC the traction water without added acid, bases, or other chemical reagents that you want to retrieve. This means that less dry matter is transferred from raw materials in the liquid fraction (extract)than in most other ways of pre-processing.

Transfer hemicellulosic sugars usually will be less than 60%, and lignin - less than 20% of the initial content in raw materials. Hemicellulose is hydrolyzed, but mostly in the oligomers and soluble polymers, which can hydrolyze further enzymes with getting able to fermentable sugars.

Refusal adding acids means low formation of fermentation inhibitors. In addition, small amounts of inhibitors will concentrate in the liquid fraction from pre-treatment, if you need low-cost to spend detoxification. Detoxification, if needed, for the method according to the invention preferably is carried out using NH3.

Refusal adding acids, bases or other chemicals that you want to extract, also leads to lower operating costs.

One the first stage of hydrothermal pre-treatment (HTP) may contain soaking, which can be done in containing acetic acid liquid fraction with later stage at atmospheric pressure and temperatures up to 10°C. The purpose of soaking is to displace air from the raw material and to ensure saturation of the whole raw material liquid. Another goal is to use part of the energy of the liquid fraction to raise the temperature of the raw material. The following objectives of the stage soaking is to increase the dry matter content of the liquid fraction and soak raw organic acids formed in the following steps.

The next step might be handling high pressure at temperatures from 100°C to about 230°C, carried out, for example, as the process of ideal displacement and high percentage of the solid phase.

In order to achieve the desired economic benefits, at least stage hydrothermal pre-treatment (HTP), carried out at high pressure should preferably take place with a high concentration of solid dry mass in the reactor. Thus, the reactor preferably 100%full and voluminous raw materials provides this option, as the seal. Often a cost-effective solution reactors are continuous with a high content of dry solids, based on the helical device, but in the case of a 100%fill transporting function screw devices may not be enough. Therefore, embodiments of the reactor can include devices with two vzaimozavisimy the I screws or device with a single screw reciprocating axial movement.

A high concentration of solid dry mass in the reactor is achieved in a flow system, as described in patent US 5503996 (Torget), where the fluid flows in a flow system relative to the solid phase that is not suitable for most embodiments of the second aspect of the present invention. Instead, in preferred embodiments of the second aspect of the present invention uses a system of soaking/spin. In this context, soak it implies that the empty volume of the solid is completely filled with liquid and the extraction implies that most of the liquid is again removed. The ratio of solid dry mass to liquid when the soaking should be as large as possible to obtain a high concentration of dry matter in the liquid.

When the transfer of biomass from the stage, soaking in the subsequent processing high pressure biomass preferably remove the water to reduce the energy required to raise the temperature of the biomass to the level of the stage hydrothermal pre-treatment (HTP), carried out at high pressure. The temperature can be achieved by adding hot water and/or steam. Raw materials can be subjected to the action of shear forces in the conditions of high temperature to release soft lignin from cellulose. Shear forces can be applied is different which means, for example transporting device in the reactor, a device driven conveyor device, or by pressing at the loading and unloading of the reactor. Shear forces can also be directed through a steam explosion, which consists mainly in the rupture of cells and capillaries. Tool application shear forces can be applied independently or in combination of two or more funds.

The concentration of solid dry mass when the soaking will typically be 10-20%, and after wringing 30-40%, so approximately 2.5-3.5 kg of fluid per kg dry solid mass is added when the soaking and again removed during the spin cycle.

Each stage of maceration and extraction can transfer the dry material from a solid into a liquid fraction.

One purpose of hydrothermal pre-treatment (HTP) is to make the cellulose available for enzymatic hydrolysis/attack. The specific purpose is not the removal of hemicelluloses and lignin from the solid fraction, and the neutralization of their protection of the pulp. Currently, it is believed that when the lignin melts in the presence of water, the hydrophobic lignin will form droplets, which are dried at low temperatures to form microparticles without any or with very slight protective effect against cellulose. In the conditions which x the melting of lignin during the hydrothermal pre-treatment (HTP) hemicellulose will be either hydrolyzed to such an extent, when it no longer protects the cellulose from the attack of enzymes. It is also believed that the melting conditions of lignin will fade the crystallinity of cellulose, which is crucial for the achievement of efficient enzymatic hydrolysis. To improve the allocation of molten lignin from the cellulose fibers, the raw material is subjected to the action of shear forces. They will tear lignite from cellulose and facilitate the formation of free droplets of hydrophobic lignin. Drops, apparently, will be covered with a hydrophilic compounds obtained mainly from partially hydrolyzed hemicelluloses. It was unexpectedly found that the resulting microparticles lignin does not have any inhibitory effect on obtaining ethanol fermentation yeast-based or thermophilic compounds, fermenting C5-C6, developed by the company TMO Biotec Ltd, Guildford, UK.

One of the problems of industrial continuous pre-treatment of bulky raw materials with a high concentration of long particles is the transfer of raw materials in the reactor pressure vessels in a safe, efficient and reliable way. It is advantageous to load raw material into the reactor portions using the boot device gateway type, such as a pump for the crushed material, described in WO 03/013714A1, and at any time at least one pneumatic is ATOR provides a tight seal between the reactor pressure vessels and vats for maceration. This pump is for the crushed material can remove the liquid from the soaked raw materials by extraction when loading into and unloading from the reactor and discharging can be combined with a steam explosion.

According to one variant of implementation of the second aspect of the present invention carried out at high pressure stage hydrothermal pre-treatment (HTP) can be implemented with one or more sets of conditions temperature/pressure. The transfer of materials from one zone of high pressure to another will normally be held device pressed through a gateway system. Additional operations of extraction/soaking may be carried out in each zone of high pressure.

Pre-treated raw material can be squeezed when it is still in a high temperature environment with lignin in the form of droplets, or it can do push-UPS after it is unloaded from the reactor hydrothermal pre-treatment (HTP) with lignin in the form of solid particles.

One advantage of the wringer before unloading of raw is that you can get a higher dry matter content in the solid fraction (TF), is possible without excessive drying. Another advantage of pressed under high pressure and temperature is that the shear forces generated during the spin cycle, will provide superior you shall order his drops of lignin. One advantage pressed at temperatures below 100°C is that costs are reduced, and that more lignin remains in the solid fraction.

The pressure relief as solid and liquid fractions can be carried out in closed systems without access of air to collect the emitted pairs and use thermal energy of steam in order to concentrate condensate as process water.

In order to obtain an effective enzymatic softening, it is desirable to place as many of the enzymes on the surface of the pulp fibers contained in the particles pre-treated solid fraction (TF). To achieve this, warm pressed solid fraction (TF) is mixed with colder enzyme drug that can be absorbed in the cavity of the particles. Couples captured in the cavity, condenses when cooled enzyme preparation, and creates a vacuum, pulling the enzyme preparation in the cavity. Selecting the concentration of the enzymes in the product, you can put the desired number of enzymes on the inner and outer surfaces of the particles adhering to the cellulose fibers. Due to such adherence of the dry matter content in full of the enzymes of the solid fraction (TF) can be increased by pressing, at the same time preventing removal of enzymes to an unacceptable level.

R is huirua the temperature and pH of the enzyme preparation before mixing with the warmer pre-treated TF, you can obtain the optimum conditions of the tender.

According to Tolan, enzymes for hydrolysis of cellulose should typically contain three types of enzymes: endoglucanase, cellobiohydrolase and beta-glucosidase. The first two hydrolyzing a polymer cellulose to soluble dimeric cellobiose, which is then hydrolyzed to glucose by the enzyme of the third type. Inhibition by product cellobiose and glucose can be prevented or reduced by increasing concentrations of beta-glucosidase and use separate hydrolysis and fermentation. Another solution is to use a process of simultaneous saccharification and fermentation (SSF), and cellobiose and glucose into ethanol by the action of the fermenting organism. One variant of implementation of the present invention is based on the successful establishment of thermophilic ethanologenic microorganisms, which are able to ferment sugars C5 and C6, and a compatible enzyme systems with high activity hemicellulase and cellulase at temperatures around 60°C and at a pH of about 6. Of particular interest to the present invention are thermophily with the ability to ferment not only monomers but also small oligomers, such as cellobiose, maltose and raffinose, which, together with a compatible enzyme the system will create the ideal solution for the th process of simultaneous saccharification and fermentation (SSF) for the conversion of pretreated according to the invention of biomass to ethanol. Alternatively, the method according to the invention can use the approach in which is introduced a separate stage softening, which gives optimal conditions for the enzyme activity, followed by the process of simultaneous saccharification and fermentation (SSF) with softened a fraction as the substrate and with the optimum conditions for fermentation of the organism, but with suboptimal conditions for enzymes.

During softening, natalizumab, for example, cellulases Tricoderma at a pH of about 5 and a temperature of about 50°C, endoglucanase can provide basic depolymerization, as the activity of cellobiohydrolase quickly inhibited accumulated cellobiose, and the activity of beta-glucosidase is inhibited accumulated glucose.

Softening may be carried out on the basis of two principles: liquid - or solid-phase softening.

For solid-phase softening filled with enzyme fraction of fibers is transferred to a mixer, which contains no free liquid in the input area.

When solid softening at industrial scale microscopic traffic enzymes from attack to attack, the pulp may not always provided with the usual stirring, so as to overcome the friction between particles requires large power consumption. Instead, technology can be applied, using the jaś in industrial composting, for example the drums for composting, where the solid fraction (TF), filled with enzymes, undergoes a series of UPS and downs during transfer through a cylindrical drum which rotates or is stationary and is equipped with a rotor with lifting devices.

Liquid-phase softening coming, filled with enzyme particle solid fraction (TF), immersed in a viscous fluid the softened material. Even if the mixture viscosity, the mixing can be performed using various known mixing devices.

Some advantages of liquid-phase softening are:

the dry matter content in the reactor may be high,

- transfer of appropriate efforts to ensure the movement of enzymes from attack to attack cellulose, facilitated by the liquid,

- possible return softened faction with enzymes in the input area.

The reactor softening according to the present invention may have the elongated cylindrical container with an inlet for full enzyme solids (TF) in the upper part of one end of the container and the outlet for softened fraction (LfF) in the lower part of the other end of the container.

At the entrance perforated piston device may promote particle solid fraction (TF) to exit completely immersed in the softened a fraction. The output of the sieve device can separate the residual particles (PTS), consisting mainly of cellulose and lignin, softened fraction (LfF), consisting mainly of mud softened polysaccharides and particulate lignin. When passing through the reactor structure most (TF) particles will gradually disappear, and the residual particles (PTS) you can sort, split and return to the reactor inlet.

Mixing of the reactor may be suitable mixing devices, and may optionally be applied vibration using oscillations with a wavelength of from a few millimeters to the wavelength of the ultrasound. After removal of the residual particles (PTS) of the LfF microparticles lignin can be removed on a tray and frame filter with getting the filter residue with a dry matter content of up to 70%, thanks to that achieved low costs for drying. This product usually has a low content of KCl and therefore can be burned in power plants with high electricity output. The filtrate can be stored in the supply tank, where the temperature, pH and nutrient content can be adjusted to optimize the conditions of the subsequent process of simultaneous saccharification and fermentation (SSF). If the process of simultaneous saccharification and fermentation (SSF) is based on the yeast, the temperature should be lowered to about 35°C and pH 5, you can leave

If the process of simultaneous saccharification and fermentation (SSF) is performed on the basis of thermophilic microorganisms, fermentation C6 and C5, such as thermopile company TMO Biotec, the temperature may be increased to about 60°C and pH to about 6.

This process of simultaneous saccharification and fermentation (SSF) can be conducted as a batch or continuous process, depending on the equipment, which is in itself known.

Removing the ethanol can be carried out by the usual method of rectification.

The preferred technology of extraction of the present invention is the use of technology distillation, such as vacuum distillation, gas cleaning, or evaporation, by sputtering, in which the temperature of the fermentation mixture will remain close to the temperature of the fermentation when the removal of ethanol.

Thereby limited by thermal inaktivirovanie enzymes and fermenting organisms, thus, enzymes and fermenting organisms may be returned in a cycle to produce further cost savings.

Microparticles lignin can during fermentation to stay in the softened faction, as microparticles macromolecular lignin does not have any inhibitory effect. Simultaneous fermentation of obtaining ethanol and the extract is interesting, to decrease the non cost option for the method according to the invention, moreover, the ethanol is removed before the inhibition will begin to slow down fermentation. Removing the ethanol by fermentation can be carried out by distillation gas with application of the principle of evaporation by spraying, in which ethanol can be removed from the fermentation mixture without heat inhibition of enzymes and microorganisms that can be returned to the fermenter.

Technological scheme of Fig. 1-3 illustrate various examples of preferred embodiments of this method of transformation.

In Fig. 1 shows the conversion of baled straw and grain in a situation where competition fermentation of C5 and C6 sugars by Thermopylae too low. Therefore, C5 and C6 sugar released from the solid fraction (TF) of straw, combined with the C6-sugars in the grain and subjected to yeast fermentation. In ethanol become only the C6-sugars. C5-sugar increase the proportion of soluble dry matter in Barda and together with the C5-sugars liquid fraction (state) going in DDGS.

Fig. 2 illustrates an implementation option, in which thermophilic fermentation can compete with yeast, when mixed sugar C5 and C6, but not by pure fermentation of C6. In addition, a compatible system of thermoflow and enzymes are not ready for industrial application. So there are two different fermentation. The permeate from the ultrafiltration of liquid fraction (state) and what is to replace the water in the grout grain, in the embodiment, with Fig. 1.

A solution of ethanol processing straw concentrate and dehydrated in the process of grain processing.

In Fig. 3 shows an implementation option that includes only thermophily, fermenting sugar C5 and C6. As for straw and grain require different systems of enzymes, there are two separate process of simultaneous saccharification and fermentation (SSF). The process of simultaneous saccharification and fermentation (SSF) of the straw is carried out at lower temperature and pH than the process of simultaneous saccharification and fermentation (SSF) of grain to align with the requirements of the enzyme system. The liquid fraction is fed directly to the process of mashing the grain.

It should be understood that all the above in connection with the invention of distinctive features and achievements according to the second aspect of the invention and variants of its implementation applicable to the above-discussed first aspect of the invention and/or to variants of its implementation.

1. Method for continuous hydrothermal pretreatment of lignocellulosic biomass for ethanol without the addition of acids, bases or other chemicals that must be removed, including:
(i) soaking, which can be done in containing acetic acid fluid with subsequent stage hydrothermal pre the preliminary processing, with the exclusion of air from lignocellulosic biomass, the receipt of all raw materials, saturated liquid and saturated lignocellulosic biomass organic acids formed in the subsequent stages, and the subsequent
(ii) continuous hydrothermal pre-treatment under pressure of the material at a temperature of from 170 to 200°C,
where lignocellulosic biomass is a corn stalks, chopped whole plant and the pulp,
where the pre-processed raw materials then wring out there under pressure or after unloading from the reactor pre-treatment with obtaining fractions of fibers and liquid fractions, and
where the temperature and duration of the hydrothermal pre-treatment is chosen so that the transition hemicellulosic sugars from lignocellulosic biomass into a liquid fraction of at least 60% of the initial content of lignocellulosic biomass, and that more than 80% of the initially contained in the lignocellulosic biomass lignin remained in the fraction of fibers, which then undergoes enzymatic softening and saccharification.

2. The method according to claim 1, further characterized by the collection of gas separated from the process of hydrothermal pre-treatment, and its use in evaporation processes.

3. The method according to claim 1, in which at least cha is th or fraction liquid fraction is used to reduce the dry matter content in sugar and/or starch raw material of the production of ethanol, based on starch and/or sugar, such as the process of mashing the grain.

4. The method according to claim 1, in which cellulosic biomass is cleaned from sand, stones and other unwanted heavy objects by wet cleaning using a liquid fraction, such as wash water.

5. The method according to claim 1, further characterized in that the softening fraction of the fibers are dipped fraction of fibers filled with particles of the enzyme, in a viscous fluid the softened material.

6. The method according to claim 1, further characterized by simultaneous saccharification and fermentation (SSF) fermentative softened fraction of fibers for ethanol production.

7. The method according to claim 1, further characterized in that the enzymatic softening fraction of fibers is held in a cylindrical drum, equipped with a rotor with lifting devices.

8. The method according to claim 6, characterized in that the method of producing ethanol is associated with the existing power plant.

9. The method according to claim 6, further characterized by the fact that SSF unite with the process of distillation of alcohol, in which the temperature during the removal of the ethanol avoids thermal inactivation of enzymes, which allows you to return the enzymes in the cycle.

10. The method according to claim 6, characterized by the fact that SSF unite with the process of distillation of the alcohol, based on g is zociste.

11. The method according to claim 6, characterized in that the microparticles of the lignin is obtained from a mixture of SSF, which is suitable for co-firing solid fuels with coal dust.

12. The method according to claim 6, characterized in that the ethanol product is combined with ethanol product process based on starch and/or sugar.

13. The method according to claim 6, further characterized in that the microparticles remain lignin in the enzymatic mixture.

14. The method according to claim 1, where at least a part or fraction liquid fraction is used to retrieve the feed for ruminant animals.

15. The method according to claim 1, where at least a part or fraction liquid fraction is used as raw material for ethanol production.

16. The method according to claim 1, characterized in that the microparticles of the lignin receive so that they are suitable for co-firing solid fuels with coal dust.

17. The method according to claim 1, wherein the fibrous structure of lignocellulosic biomass is saved.

 

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