WO2012066042A1 - Mesures dans le pir dans la production d'un agent chimique cible à partir de cellulose - Google Patents

Mesures dans le pir dans la production d'un agent chimique cible à partir de cellulose Download PDF

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Publication number
WO2012066042A1
WO2012066042A1 PCT/EP2011/070264 EP2011070264W WO2012066042A1 WO 2012066042 A1 WO2012066042 A1 WO 2012066042A1 EP 2011070264 W EP2011070264 W EP 2011070264W WO 2012066042 A1 WO2012066042 A1 WO 2012066042A1
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slurry
arrangement
nir
pretreatment
fermentation
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PCT/EP2011/070264
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Elias Sundvall
Torbjörn VAN DER MEULEN
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Sekab E-Technology Ab
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
    • C12M41/00—Means for regulation, monitoring, measurement or control, e.g. flow regulation
    • C12M41/26—Means for regulation, monitoring, measurement or control, e.g. flow regulation of pH
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
    • C12M41/00—Means for regulation, monitoring, measurement or control, e.g. flow regulation
    • C12M41/30—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration
    • C12M41/32—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration of substances in solution
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/02—Monosaccharides
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
    • C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N2021/8411—Application to online plant, process monitoring
    • G01N2021/8416—Application to online plant, process monitoring and process controlling, not otherwise provided for
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the present invention relates to methods for process control.
  • the invention relates to control of processes of production of target chemicals from cellulosic biomass.
  • Biorefineries producing green chemicals, such as bioalcohols, from renewable resources offer an alternative to oil refineries based on dwindling supplies of petroleum and permit a move towards improved energy security.
  • Lignocellulosic residues from forestry and agriculture are attractive as feedstocks, since they are abundant, relatively inexpensive, and are not used for food.
  • Lignocellulose consists mainly of lignin and two classes of polysaccharides, cellulose and hemicellulose. The polysaccharides can be hydrolyzed to sugars and converted to various fermentation products, such as bioalcohols, in processes based on biocatalysts, such as the industrially important baker's yeast (Saccharomyces cerevisiae).
  • the hydrolysis of cellulose is typically preceded by a pretreatment, in which the hemicellulose is degraded and the cellulose is made increasingly accessible to cellulolytic enzymes.
  • hydrolysis and fermentation can be performed simultaneously in a simultaneous saccharification and fermentation (SSF) process or in a consolidated bioprocess (CBP).
  • SSF simultaneous saccharification and fermentation
  • CBP consolidated bioprocess
  • SHF separate hydrolysis and fermentation
  • Saccharification and hydrolysis are synonymous and used interchangeably in the present disclosure.
  • a major challenge in processes involving hydrolysis of cellulose and fermentation of the hydrolyzate is to reduce costs such that the produced products may compete with products produced with traditional processes.
  • Summary of the present disclosure The process of production of target chemicals, such as bioalcohols, from cellulosic biomass can involve several different consecutive process steps, such as a pretreatment step, a hydrolyzing step and a fermentation step. To get an efficient process and a high yield of product it is important that the process is accurately monitored and controlled.
  • One well established way of monitoring and controlling a process for production of target chemicals from cellulosic biomass involves manually taking out samples at specific process steps (e.g. at the pretreatment step, the hydrolyzing step or the fermentation step) and analyzing the chemical properties of the samples taken at these process steps in the laboratory to generate a value of the measured property.
  • the value can be compared with a reference value and based on the comparison the analyzed process step can be adjusted by changing process parameters of the process step.
  • the present inventors have thus realized that there is a need for improved methods of regulation of processes of production of target chemicals from cellulosic biomass.
  • both the material from the pretreatment step and the material in the separate or simultaneous saccharification and fermentation process shall be analyzed.
  • the inventors have further realized that the control of a process for production of target chemicals from cellulosic biomass is improved if the results of both the analyses are used to determine how to control (a) process parameter(s) of the pretreatment process and/or the saccharification and fermentation process.
  • analysis of the material from the pretreatment step gives information about the performance of the pretreatment step and about the characteristic of the material entering the hydrolysis or SSF step. By combining this information with information gained by analyzing the material in the hydrolysis and fermentation, it is easier to determine which process parameters that need to be adjusted and to what level.
  • the inventors have also realized that due to variations in the feedstock and to the unpredictable behavior of the enzymes and micro-organisms, changes in process parameters often need to be swift in order to save and or correct an ongoing process. Therefore the inventors have come to the conclusion that the manual sampling methods and subsequent laboratory analyses described above often are too time consuming to be suitable in a method of controlling processes of production of target chemicals from cellulosic biomass. Manual sampling methods can not be used for online measurements and the changes in process parameters based on the measurements can not easily be made automatic. The inventors have thus realized that there is a need for a fast detection method which preferably can be used for continuous online (e.g. real-time) measurements in the different process steps and which can be used for a quick adjustment of process parameters.
  • a fast detection method which preferably can be used for continuous online (e.g. real-time) measurements in the different process steps and which can be used for a quick adjustment of process parameters.
  • Spectral analysis is widely used in different fields of technology. In chemistry, spectral analysis is used for analyzing the chemical properties and composition of a material. The material is often first subjected to light or radiation which is thereafter either absorbed or reflected. Depending on the degree of absorption and/or reflection at specific wavelengths, specific to the material under investigation, a spectrum is obtained which may be analyzed to identify or characterize the material.
  • NIR Near Infrared spectroscopy
  • the Near Infrared spectroscopy is hereinafter referred to as only NIR.
  • NIR uses the wavelength range immediately beyond the visible range, i.e. 750 - 2500 nm, and has the advantage that it is able to penetrate material.
  • NIR is a fast and accurate analysis method and in the present disclosure the inventors have demonstrated that NIR can be used for online
  • the inventors Since the measurements can be performed online, the inventors have realized that it is possible to automatically adjust various process parameters based on the online measurements. This enables an even faster adjustment of process parameters which makes the process control more effective.
  • NIR is a particularly useful analysis method for monitoring and control of processes for production of target chemicals, from cellulosic biomass.
  • the present invention is partly based on the insights and findings described above and provides improved methods of controlling processes of production of target chemicals from cellulosic biomass.
  • a first aspect of the invention relates to a method of producing a target chemical from a cellulosic starting material, comprising the steps of:
  • step b) analyzing the slurry from step a) with NIR spectroscopy to obtain at least one NIR spectrum characterizing the slurry from step a) (first data set);
  • step c) subjecting the slurry from step a) to separate or simultaneous
  • a second aspect of the invention relates to a system for the
  • a pretreatment arrangement for the preparation of a slurry from the cellulosic starting material comprising an inlet and an outlet;
  • a bioconversion arrangement for saccharification and fermentation of the slurry from pretreatment arrangement to produce a fermentation broth comprising the target chemical, comprising an inlet connected to the outlet of the pretreatment arrangement and an outlet, wherein
  • a NIR spectroscopy instrument which comprises a probe and a spectrometer, is arranged to analyze slurry from a position in the connection between the outlet of the pretreatment arrangement and the inlet of the bioconversion arrangement (first position) and provide NIR data
  • a NIR spectroscopy instrument which comprises a probe and a spectrometer and may be completely or in part the same as the previously mentioned NIR instrument, is arranged to analyze slurry from a position in the bioconversion arrangement (second position) and provide NIR data
  • control device arranged to receive NIR data from the first and the second position and control at least one process parameter in the
  • pretreatment arrangement and/or the bioconversion arrangement in response to the received NIR data from the first and second position.
  • a third aspect of the invention relates to a system for the preparation of a target chemical from a cellulosic starting material, comprising:
  • a pretreatment arrangement for the preparation of a slurry from the cellulosic starting material comprising an inlet and an outlet;
  • a bioconversion arrangement for saccharification and fermentation of the slurry from pretreatment arrangement to produce a fermentation broth comprising the target chemical, comprising an inlet connected to the outlet of the pretreatment arrangement and an outlet, wherein
  • a NIR spectroscopy instrument is arranged to analyze slurry from a position in the connection between the outlet of the pretreatment arrangement and the inlet of the bioconversion arrangement (first position) and provide NIR data;
  • a NIR spectroscopy instrument which may be the same as the previously mentioned NIR instrument, is arranged to analyze slurry from a position in the bioconversion arrangement (second position) and provide NIR data;
  • control device arranged to receive and process NIR data from the first and the second position, said control device comprising a display for displaying the processed NIR data such that at least one process parameter in the pretreatment arrangement and/or the bioconversion arrangement may be controlled in response to the received NIR data from the first and second position.
  • Figure 1 A NIR-measuring probe is installed directly in a process pipeline. It is placed near a manual sample point to be able to take out reference samples for calibration.
  • Figure 2 Total sugar concentration in pretreated lignocellulosic material. The x-axis shows the concentration predicted by the NIR instrument and the Y- axis shows the concentration from the laboratory analysis.
  • Figure 3 In this example the glucose content is separated from the rest of the sugars.
  • the x-axis shows the concentration predicted by the NIR instrument and the Y-axis shows the concentration from the laboratory analysis.
  • Figure 4 Ethanol concentration in hydrolyzate from a fermentation vessel in a demo-scale cellulose ethanol plant.
  • the x-axis shows the concentration predicted by the NIR instrument and the Y-axis shows the concentration from the laboratory analysis.
  • Figure 5 Dry substance content in hydrolyzate from the pre-treatment step.
  • the x-axis shows the concentration predicted by the NIR instrument and the Y-axis shows the concentration from the laboratory analysis.
  • Figure 6 Amount of suspended solids (SS) in hydrolyzate from the pre- treatment step.
  • the x-axis shows the concentration predicted by the NIR instrument and the Y-axis shows the concentration from the laboratory analysis.
  • Figure 7 shows the control of a system/method involving separate
  • Figure 8 shows the control of a system/method involving simultaneous saccharification and hydrolysis.
  • a first aspect of the invention relates to a method of producing a target chemical from a cellulosic starting material, comprising the steps of:
  • step b) analyzing the slurry from step a) with NIR spectroscopy to obtain at least one NIR spectrum characterizing the slurry from step a) (first data set);
  • step c) subjecting the slurry from step a) to separate or simultaneous
  • pretreating refers to modifying the cellulosic starting material to make the cellulose therein more accessible to hydrolytic activity in the subsequent hydrolysis.
  • the pretreatment may be acidic pretreatment or alkali pretreatment.
  • the pretreatment may be aided by the addition of a catalyst.
  • the catalyst may be added as a fluid in an impregnation step, which is followed by a heating step. The heating is normally achieved by the addition of steam.
  • the fluid may be an acidic solution, such as an aqueous mineral acid solution, such as sulfuric or sulfurous acid.
  • the impregnation may also be performed with a gas, such as a SO2 gas or CO2 gas, or with the combination of a gas and a liquid.
  • the pretreatment may also comprise steaming. Steaming refers to a process used to drive air out from the cellulosic biomass to facilitate further hydrolysis of the cellulose. Steaming is a well-known method for pretreating e.g. lignocellulosic biomass.
  • the pretreatment may involve steam explosion. Steam explosion is a process that combines steam, rapid pressure release and hydrolysis for rupturing cellulosic fibers. Steam explosion may be performed with or without a preceding addition of a catalyst,
  • the method according to the first aspect enables an efficient control of the process and therefore the method has several advantages compared to other methods described in the art.
  • the analysis of the material in step b gives information about the performance of the pretreatment step and about the characteristic of the cellulosic material entering the hydrolysis/SSF step (step c).
  • the analysis in step d gives information about the characteristic of the cellulosic material in the hydrolysis and fermentation step. By combining this information, the process parameters that need to be adjusted can be determined.
  • the use of NIR for measurements in these two positions enables an accurate analysis method which can be used for online measurements of several important properties needed for an efficient monitoring and control of processes of production of target chemicals from cellulosic biomass.
  • any suitable process parameter of the pretreatment process and/or saccharification and fermentation process can be controlled in response to the first and the second data set.
  • an effective pretreatment is needed to liberate the cellulose from the lignin seal and its crystalline structure so as to render it accessible for the subsequent hydrolysis step. If the pretreatment is not harsh enough, it will be harder to hydrolyse the carbohydrates to sugars. However if the pretreatment is too harsh larger amounts of sugars will be degraded and fermentation inhibitors such as HMF, furan aldehydes (e.g. furfural), acetic acid and/or phenolic compounds will be formed, which in turn might impair the hydrolysis and/or fermentation process. It is therefore important to control the severity of the pretreatment. The most important severity parameters of the pretreatment process reaction is the pH, the temperature, the pressure and residence time of the cellulosic material in the pretreatment process.
  • the process can preferably be controlled by addition of a detoxification agent which counteracts the negative effect of the inhibitors on the hydrolysis and/or fermentation process.
  • a detoxification agent which counteracts the negative effect of the inhibitors on the hydrolysis and/or fermentation process.
  • Preferred examples of such a detoxification agent include but are not limited to reducing agents such as dithionite and sulphite.
  • the reducing agents may be added directly to the saccharification and/or fermentation process.
  • Other detoxification agents, such as alkali are normally added in a separate step such that the pH may be adjusted to a level suitable for hydrolysis and/or fermentation afterwards.
  • Other examples of detoxification agents may include enzymes such as for example laccase.
  • the saccharification and fermentation process is infected by other microorganisms such as bacteria. This is undesired for several reasons.
  • the infecting microorganism might compete with the fermenting agent for the sugars and convert sugars to undesired chemicals instead of the desired target chemicals. If the saccharification and fermentation process is infected by other microorganisms the process can be controlled by addition of an agent which is toxic to the infecting
  • the fermenting agent is yeast and the saccharification and/or fermentation process is infected by bacteria, the process can be controlled by addition of an antibacterial agent, such as an antibiotic, such as VitaHop®.
  • an antibacterial agent such as an antibiotic, such as VitaHop®.
  • bacteria that might infect a fermentation process is lactic acid bacteria that produce lactic acid from available saccharides.
  • the process can preferably also by controlled by regulating a slurry feeding rate in the saccharification and fermentation process.
  • a slurry feeding rate in the saccharification and fermentation process.
  • the feeding rate of the slurry into the saccharification and fermentation process can be adjusted so that the concentration of the inhibitors is not higher than what yeast or other microorganisms employed can handle.
  • the feeding rate can also be adjusted such that the levels of carbohydrates and sugars are optimal for the enzymes and the fermenting agent in the saccharification and fermentation process.
  • the feeding rate can also be adjusted to maintain the SS content (i.e. viscosity) at a desirable level.
  • Variation in temperature or pH, infections, or high levels of inhibitors can have severe effect on the fermenting organism and/or the enzymes in the fermenting and saccharification process.
  • the fermenting agent for some reason is dying or working less well, it might be necessary to control the process by addition of more fermenting agent to the fermenting or SSF step.
  • the activity of the enzymes decreases, it can also be necessary to control the process by addition of more enzymes to the saccharification or SSF step.
  • the saccharification and fermentation process might work less efficient if the dry solids content (or suspended solids) and thus the viscosity is too high. Water can be added to the process to decrease the dry solids content (or suspended solids). High levels of sugars in the hydrolysis step leads to end-product inhibition. To counteract this inhibition the hydrolysis reaction can be diluted with water.
  • Saccharification and fermentation processes can also be diluted with water to decrease the concentration of inhibitors and other toxic substances.
  • the process can be controlled by addition of an amount of water in the saccharification and fermentation process.
  • the added water can for example be pure water or recycled process water. It is also beneficial to be able to control when to terminate a saccharification and fermentation process. For example it might be beneficial to terminate the process when the level of remaining sugar and/or carbohydrates is below a certain value or when the concentration of the target chemical has reached a certain level.
  • At least one process parameter of step e) is selected from the group consisting of:
  • a slurry feeding rate in the saccharification and fermentation process an amount of enzymes added in the saccharification and fermentation process
  • step b) and d) are compared with a reference data set.
  • a single reference data set might be a set point value which preferably is an interval or a range consisting of a minimum and a maximum value. Such ranges are preferably established for a host of process data sets, which can be combined as a matrix to create a process window in which the process should be remained. If measured values fall outside the process window, process parameters can be controlled to adjust the process.
  • process data sets are preferably NIR-based data sets but other types of process data can also be used to establish the process window. Therefore, in one embodiment step b) and d) further comprise comparing the first and the second data set with reference data and step e) comprises controlling the at least one process parameter in response to differences between the data sets and the reference data.
  • a NIR-spectra contains hundreds of variables and therefore some kind of multivariate data analysis method is preferably used to analyze raw data from the measurements.
  • multivariate data analysis methods are well known in the art and includes Partial least squares regression (PLS); PLS Discriminant Analysis (PLS-DA); Ordinary Least Squares (OLS) regression; MLR (multiple linear regression); OPLS (Orthogonal-PLS); SVM (support vector machines); GLD (general discriminant analysis); GLMC (generalized linear model); GLZ (generalized linear and non-linear model); LDA (Linear Discriminant Analysis); classification trees; cluster analysis;
  • Steps b) and d) (and step aa), if applicable, see below) may
  • step e) may comprise time correlating the data sets and controlling the at least one process parameter in response to time correlated data sets.
  • the causal connection of process parameters and slurry characteristics can be determined.
  • the conditions at one stage of the process may be linked to the conditions of another, earlier stage of the process.
  • parameter of the saccharification and fermentation process may be based on a concurrent/real-time analysis of the slurry in the saccharification and fermentation process and a previous analysis of the slurry from the
  • the recorded time points may be used for calculating the derivative of a process parameter derived from the data sets.
  • the derivative of the ethanol concentration in the fermentation process may be calculated. If the ethanol concentration derivative is close to zero, one of the following actions may be taken depending on the results of other analyses: addition of more fermenting agent (e.g. yeast) to the fermentation process; addition of detoxification agent to the fermentation process; addition of an antibacterial agent to the fermentation process;
  • step e) may comprise controlling the at least one process parameter in response to data obtained in steps b) and d) (and step aa), if applicable, see below) over a period of time.
  • control may be in response to mean, median or derivative values derived from a plurality of analyses in steps b) and d) (and possibly aa)), respectively.
  • parameters which preferably can be determined with NIR in step a) or c) include total concentration of monomeric sugars.
  • Measurements of total monomeric sugar in step a) gives information about the severity of the pretreatment; typically, a high concentration of total monomeric sugars in step a) indicate high severity of the pretreatment whereas low concentration indicates low severity. However, at very harsh pretreatment conditions the total monomeric sugar levels decreases due to high levels of sugar degradation in the process.
  • the measurement of total monomeric sugar in step a) also gives information about the amount of monomeric sugars that is going into the saccharification process or the SSF process. Measuring of the amount of total monomeric sugars in the
  • step c gives information about how fast monomeric sugars are produced in the hydrolysis step and about how fast the sugars are consumed in the fermentation step.
  • Information about the concentration of total monomeric sugars is particularly useful in a process using a fermenting agent capable of fermenting both hexoses and pentoses.
  • Many of the fermenting agents currently used in industrial processes for production of ethanol are capable of utilizing hexoses but are not very efficient in utilizing pentoses. Therefore, it might be preferred to measure the concentrations of at least one hexose monosaccharide, such as glucose, mannose and/or galactose.
  • a fermenting agent that utilizes pentoses is used, optionally in combination with a yeast that utilizes hexoses, the concentration of at least one pentose monosaccharide, such as xylose, can also be measured.
  • decomposed sugars and fermentation inhibitors such as e.g. furfural, hydroxymethylfurfural), acetic acid and/or phenolic compounds in step a) gives information about the severity of the pretreatment. This is thus valuable information which can be used to control the pretreatment process.
  • Information about the levels of fermentation inhibitors in step a) is also valuable information which can be used in the regulation of the feeding of pretreated material into the saccharification and fermentation step. Based on this information, in combination with information about the concentration of fermentation inhibitors in step c), the feeding rate of the slurry into the saccharification and/or fermentation process can be adjusted so that the concentration of the inhibitors is not higher than what yeast or other microorganisms employed can handle. Also, if higher levels of inhibitors are detected, their inhibiting effect may be counteracted by the addition of one or more detoxification agents.
  • the saccharification and fermentation reaction can be infected by for example bacteria and such an infection can be combated by addition of antibacterial agent. Therefore it is highly desired that infections can be detected.
  • Some bacteria produce lactic and thus high levels of lactic acid can be an indication of an infection.
  • High levels of glycerol can be an indication of that there is some thing wrong with the fermenting agent (e.g. yeast).
  • the suspended solids concentration is high (causing a high viscosity) in the saccharification and/or fermentation and the concentration of inhibitors in the slurry supplied from pretreatment is also high, it may be appropriate to dilute the slurry with water or feed substrate at a lower rate. If the suspended solids concentration is lower, it may however be more appropriate to add a detoxification agent when the level of inhibitors is high in the slurry from the pretreatment.
  • the NIR-based analysis determines one or more of the following characteristics:
  • pentose monosaccharide such as xylose and arabinose
  • one or more fermentation inhibitors such as HMF e.g. furfural, acetic acid and/or phenolic compounds
  • step c) analyzed with NIR
  • spectroscopy is a slurry subjected to fermentation or simultaneous
  • the quality of the feedstock may vary, for example over different seasons, storage time and amounts of waste wood.
  • the properties of the feedstock going in to the process can also vary during a process. This is in particularly true in a continuous process where different feedstock or feedstock with different characteristics is fed in to the process. For example the water content in the feedstock might suddenly change. This change might for example affect the pre-treatment which in turn might affect the subsequent steps in the process.
  • the present inventors have realized that the process control of methods of producing target chemicals from cellulosic starting materials can be further improved if the properties of the feedstock are analyzed prior to the pretreatment. The inventors have demonstrated that NIR is suitable for this analysis. Gained information about the properties of the feedstock facilitates a quick adjustment of the conditions of the pretreatment reaction and/or the following saccharification and fermentation processes. Therefore, in a preferred embodiment the method further comprising the step of:
  • step aa analyzing the cellulosic starting material supplied to step a) with NIR spectroscopy to obtain at least one NIR spectrum characterizing the material supplied to step a) (third data set),
  • step e) comprises controlling the at least one process parameter of said pretreatment process and/or said saccharification and fermentation process in response to the first, the second and the third data set.
  • step e) further comprises comparing the third data set with reference data and step e) comprises controlling the at least one process parameter in response to differences between the three data sets and the reference data.
  • the water content of the feedstock may be measured by NIR, and if the water content is below a first reference value, moist may be added to the feedstock and/or if the water content is above a second reference value, the feedstock may be dried, e.g. by heating, or less liquid can be added to the pretreatment step.
  • a property of the feedstock can be measured by NIR and the obtained information can also be used to control the conditions of the pretreatment step.
  • NIR may be used for measuring how recalcitrant the feedstock is and the severity of pretreatment may be controlled accordingly. That is, if the material is more recalcitrant than average, more catalyst than average can be added in the pretreatment step, a higher temperature than average can be used and/or a longer residence time than average can be used.
  • How recalcitrant the feedstock is may for example correspond to the amount or proportion of hemicelluloses in the feedstock and/or the degree of crystallinity of the feedstock, and both these properties may be measured by NIR. Further, when the feedstock is a wood material, it is likely that NIR may be used for measuring the amount or proportion of bark in the material.
  • NIR may be used to measure the size of the feedstock. If necessary the feedstock can be subjected to size reduction (e.g. crushing, chopping or grinding). NIR may also be used for measuring the amount or proportion of different types of cellulosic starting materials such as the proportion of different wood species. Thus, in one embodiment the
  • the step c) is a continuous process or a fed-batch process. This can for example mean that pretreated slurry is added to the saccharification or SSF process continuously or in several steps as the process is going. If the process is continuous, liquid from the fermentation step comprising the target molecule can be redrawn from the process as the process is going.
  • the present inventors have demonstrated that NIR can be used for online monitoring of several important properties needed for an efficient control of processes of production of target chemicals from cellulosic starting materials.
  • the tern "online monitoring” means that the measurement on the slurry is performed without manually taking out a slurry sample from the process.
  • the measurement can for example take place directly in the process as it happens, for example by means of a probe inserted directly into a pipe conducting the slurry from the pretreatment or a hydrolysis and/or fermentation vessel.
  • the probe for online measurements may be arranged in connection to a sample outlet provided on such a pipe or vessel such that the measurements are performed on a sample diverted from the process.. Such a sample may be returned to the process, wasted or stored after the measurement. Since online
  • the analyzing in step b), d) and/or aa) is performed online. If the online measurements are performed very frequently, it will be possible to follow the process more or less in real-time. This will give almost immediate information about what is happening in the process and thus process parameters can be adjusted very swiftly to control the process. Therefore, in one embodiment at least one process parameter is measured frequently such as at least every minute or every thirty seconds during at least a part of the process. Said part of the process can for example be the whole process or a part of the process such as at least 10 minutes or at least 20 minutes or at least 60 minutes.
  • step e is automatic.
  • the target chemical is a fermentation product.
  • the target chemical is selected from alcohols, acids, alkanes, alkenes, aromatics, aldehydes or ketones.
  • the target chemical is selected from ethanol, butanol and succinic acid. In a preferred embodiment the target chemical is ethanol.
  • the cellulosic starting material is lignocellulosic material.
  • the lignocellulosic material can for example be a wood material such as hard wood or soft wood.
  • the wood material can for example be in the form of wood chips.
  • the lignocellulosic material can also for example be agricultural residues, such as corn cobs, corn stover, oat hulls, sugar cane bagasse or straw, (e.g. straw from barley, wheat, oat or rye).
  • the wood material can for example be spruce, pine, birch, oak or eucalyptus. Switch grass, salix and banagrass are examples of other suitable lignocellulosic biomass.
  • Step a Cellulosic material is pretreated (step a).
  • a stream of the pre- treated cellulosic material, containing a small amount of sugar, is fed in to a SSF vessel and subjected to simultaneous saccharification and fermentation (step c). If the enzymes in the SSF reactor are working properly, more sugar will be released during the reaction and the yeast will convert the sugar to ethanol.
  • step b By measuring the incoming amount of glucose in the lignocellulosic- or lignocellulosic derived material (step b) and then compare the amounts to the amounts of converted sugar in the SSF (ethanol, and by-products measured in step d), it is possible to see if the enzymes are functioning properly. If not, the process is controlled by addition of more enzymes (step e) and/or a detoxification agent.
  • Case 2 Cellulosic material is pretreated (step a). A stream of the pre- treated cellulosic material is fed in to a SSF vessel and subjected to
  • step c simultaneous saccharification and fermentation.
  • the amount of a certain yeast inhibiting or toxic chemical such as furfural is measured in the process stream going in to a SSF reactor (step b). This will be an indicator of how harsh the pre-treatment of lignocellulosic material have been. At the same time, the same inhibiting substance is measured in the SSF reactor
  • step d and the feeding rate of the incoming material may be adjusted so that the concentration of the toxic substances/inhibitors is not higher than what yeast or other microorganisms employed can handle.
  • the first measuring point (step b) is of extra help in this case because it gives information of the incoming material which allow faster process control and no overfeeding of toxic material to the SSF reactor. More material will be fed into the SSF reactor when the amount of the inhibiting substance from the measuring point inside the SSF reactor (measured in step d) is at a certain level.
  • the feed rate is controlled based on the measurement data from step b and d.
  • Case 3 Cellulosic material is pretreated (step a).
  • a stream of the pre- treated cellulosic material is fed in to a SSF vessel and subjected to simultaneous saccharification and fermentation (step c).
  • the sugar and inhibitor content is measured in the stream of lignocellulosic material from a pre-treatment step (step b).
  • the measurement shows that there is a high amount of sugar and low amount of inhibitors.
  • the second measuring point within the SSF reactor shows that the increase in ethanol content in the SSF reactor slows down and the amount of lactic acid is increasing.
  • the measurement in step b) shows that the incoming material is not the cause for the weakening of the yeast activity and hence must be caused by something inside the SSF reactor.
  • the combined information of the two measurement point indicates an infection in the SSF reactor.
  • An automatic control system adds a proper amount of biocide and then more yeast in order to control the process (step e). If the problem had been in the incoming material (e.g. high inhibitor content) the control system would suggest the addition of detoxifying chemical instead.
  • Case 4 Cellulosic material is pretreated (step a).
  • a stream of the pre- treated cellulosic material is fed in to a SSF vessel and subjected to simultaneous saccharification and fermentation (step c).
  • An online analysis in a fermentation vessel shows that the increase in ethanol content slows down and the sugar content starts to increase.
  • the online analysis of the incoming material shows that there is nothing wrong with the material going in to the fermentation vessel, hence that is not the cause of the disturbance.
  • the increasing amount of sugar in the fermenting vessel suggests that the enzymes are in good condition but the yeast has for some reason lost effect or died.
  • the control system adds new yeast to the system.
  • measurements include measuring the composition of the steam generated during pressure reduction (flashing) after pretreatment. Its composition might give valuable information on the performance of the pretreatment.
  • the steam is likely to contain components such as furfural, acetic acid, formic acid, levulinic acid, etc.
  • NIR-measurements can also preferably be used to measure the composition of the streams before and after a waste water treatment.
  • a second aspect of the invention relates to a system for the
  • a pretreatment arrangement for the preparation of a slurry from the cellulosic starting material comprising an inlet and an outlet;
  • a bioconversion arrangement for saccharification and fermentation of the slurry from the pretreatment arrangement to produce a fermentation broth comprising the target chemical, comprising an inlet connected to the outlet of the pretreatment arrangement and an outlet, wherein
  • a NIR spectroscopy instrument is arranged to analyze slurry from a position in the connection between the outlet of the pretreatment arrangement and the inlet of the bioconversion arrangement (first position) and provide NIR data;
  • a NIR spectroscopy instrument which may be the same as the previously mentioned NIR instrument, is arranged to analyze slurry from a position in the bioconversion arrangement (second position) and provide NIR data;
  • control device arranged to receive NIR data from the first and the second position and control at least one process parameter in the
  • pretreatment arrangement and/or the bioconversion arrangement in response to the received NIR data from the first and second position.
  • the control device arranged to receive NIR data from the first and the second position enables automatic control of process parameters.
  • the system according to the second aspect can preferably be used for automatic process control of such methods, wherein the process parameters can be controlled in response to the processed data without the involvement of an operator.
  • the NIR spectroscopy instrument(s) normally comprise(s) a probe and a spectrometer.
  • the probe normally has a plurality of NIR transmitting fibers each having an emitting end for emitting NIR light on the slurry and at least one receiving fiber having a receiving end for receiving reflected NIR light representative of the slurry.
  • the probe may also have a fixing material arranged to fix the fibers relative to each other and/or a probe head being arranged to assembly the receiving end(s) and the transmitting ends.
  • the receiving ends and the transmitting ends and, if applicable, the fixing material are preferably arranged to form a planar face. Thus, they may form a planar head of the probe head.
  • At least one receiving fiber may be arranged to receive backscattered NIR light from the slurry.
  • At least one receiving fiber may also be arranged to receive reflected transmittance NIR light from a reflection plate, wherein the transmittance NIR light is NIR light transmitted through the slurry.
  • the probe of the NIR spectroscopy instrument for analyzing at the first position can be arranged at any position between the outlet of the
  • the probe may for example be arranged to come into contact with the slurry. However, sometimes it can be beneficial to divert a sample of the slurry to a probe arranged next to the main pipe or at a "analysis center" of the system. .
  • a centrally arranged probe may be employed for analyzing slurry samples diverted from the different positions in the system discussed herein. For example, the same probe can be used for analysis of slurry samples from the first position and the second position.
  • system further comprising a first slurry sample outlet provided on the connection between the outlet of the
  • the NIR spectroscopy instrument is arranged to analyze a slurry sample diverted through the first slurry sample outlet.
  • the probe of the NIR spectroscopy instrument for analyzing at the second position can be arranged at any position where it comes into contact with the slurry in the bioconversion arrangement. It follows from the above that in one embodiment, the system may further comprise a second slurry sample outlet provided in bioconversion arrangement, wherein the NIR spectroscopy instrument is arranged to analyze a slurry sample diverted through the second slurry sample outlet.
  • the bioconversion arrangement comprises a bioreactor for a simultaneous saccharification and fermentation (SSF bioreactor) and said second slurry outlet is provided on the SSF bioreactor.
  • SSF bioreactor simultaneous saccharification and fermentation
  • the bioconversion arrangement comprises a fermenter and said second slurry outlet is provided on the fermenter.
  • the NIR spectroscopy instrument(s) is/are operatively connected to the control device via signal lines or a wireless communication system.
  • a device for controlling the supply of a catalyst, such as an acid, to the pretreatment arrangement ;
  • a device for controlling the supply of steam to the pretreatment arrangement ;
  • a device for controlling the temperature of steam to be supplied to the pretreatment arrangement a device for controlling the temperature of steam to be supplied to the pretreatment arrangement ;
  • a device for controlling the supply of a fermentation organism in the bioconversion arrangement a device for controlling the supply of water in the bioconversion arrangement;
  • a device for controlling the agitation in the bioconversion arrangement a device for terminating the fermentation in the bioconversion arrangement;
  • a device for controlling the feed of cellulosic starting material to the pretreatment arrangement a device for controlling the feed of cellulosic starting material to the pretreatment arrangement .
  • the NIR spectroscopy instrument which may be the same as one or both of the previously mentioned NIR instrument(s), is arranged to analyze the cellulosic starting material in a position upstream of the inlet of the pretreatment arrangement (third position) and provide NIR data; and wherein the control device is further arranged to receive NIR data from the third position and control the at least one process parameter in the pretreatment arrangement and/or the bioconversion arrangement in response to the received NIR data from the first, second and third position.
  • a first probe may thus be arranged at the first position while a second probe is arranged at the second position and, if applicable, a third probe is arranged at the third position. All such probes may be connected to the same spectrometer, which is in turn connected to the control device.
  • a spectrometer is arranged at each probe, while all
  • spectrometers are connected to the control device.
  • the probe of the NIR spectroscopy instrument can for example be in the form of an immersion probe or constitute a part of a flow cell.
  • the whole process flow or a side stream of the flow can be lead through such a flow cell.
  • a third aspect of the invention relates to a system for the preparation of a target chemical from a cellulosic starting material, comprising:
  • a pretreatment arrangement for the preparation of a slurry from the cellulosic starting material, comprising an inlet and an outlet; and a bioconversion arrangement for saccharification and fermentation of the slurry from pretreatment arrangement to produce a fermentation broth comprising the target chemical, comprising an inlet connected to the outlet of the pretreatment arrangement and an outlet, wherein
  • a NIR spectroscopy instrument is arranged to analyze slurry from a position in the connection between the outlet of the pretreatment arrangement and the inlet of the bioconversion arrangement (first position) and provide NIR data;
  • a NIR spectroscopy instrument which may be the same as the previously mentioned NIR instrument, is arranged to analyze slurry from a position in the bioconversion arrangement (second position) and provide NIR data;
  • control device arranged to receive and process NIR data from the first and the second position, said control device comprising a display for displaying the processed NIR data such that at least one process parameter in the pretreatment arrangement and/or the bioconversion arrangement may be controlled in response to the received NIR data from the first and second position.
  • Example 1 The RedEye online NIR system (Eurocon Analyzer ) was installed at two different test positions locations in a demo-scale cellulose ethanol plant (EPAB/ SEKAB E-Technology, Sweden). The first position was in a buffer tank after the pre-treatment reactors and the second position was in a fermentation vessel. The RedEye was calibrated using samples from the process and then used to analyze sugar, ethanol, inhibitor and moisture content. The RedEye base module containing spectrometer, PC-computer, electronics etc. was installed near the sample position and was connected via an optical fiber to a measuring probe. The probe was mounted directly in the process pipe using tube fitting.
  • Figure 1 shows a schematic of the installation in the process. To calibrate the instrument, a number of manual samples were taken from the process through the manual sample point. The RedEye instrument was set to save calibration spectrum as the manual sample valve was opened.
  • the reference samples from the process were analyzed in laboratory using High Performance Liquid Chromatography (HPLC). Each sample was analyzed for total sugar (arabinose, galactose, glucose, mannose and xylose), ethanol and moisture content. To develop a calibration for the instrument, the NIR-spectra, containing hundreds of variables, was combined with the HPLC results from the laboratory. To do this a Partial Least Squares (PLS) model was developed with the NIR-spectra as X-matrix and
  • the system 1 comprises a pretreatment arrangement 2 and bioconversion arrangement 3.
  • An outlet of the pretreatment arrangement 2 is connected to an inlet of the bioconversion arrangement 3, preferably via a pipe, such that slurry from the pretreatment may be supplied to the hydrolysis reaction in the bioconversion arrangement.
  • the pH of the slurry from the pretreatment may have to be adjusted, in particular if a catalyst was added in the pretreatment (see below).
  • a device e.g. vessel, not shown
  • pH adjustment may thus be arranged between the
  • the pretreatment arrangement 2 may for example comprise an impregnation chamber 21 for impregnating a cellulosic material with a catalyst and a pretreatment reactor 22 for heating the impregnated material under elevated pressure.
  • a feeding device 23 may be arranged to feed the cellulosic starting material to the pretreatment arrangement 2.
  • the feeding device 23 may for example comprise a screw, such as a plug screw.
  • a device 26 for controlling the supply of the catalyst to the impregnation chamber 21 may be arranged at the impregnation chamber.
  • the impregnation chamber 21 may thus be provided with a catalyst inlet to which the device 26 is connected,
  • the catalyst may for example be a gaseous catalyst, such as SO2 (g) or CO2 (g), or a liquid catalyst, such as an aqueous solution of a mineral acid (e.g.
  • the device 26 preferably comprises a valve.
  • Another feeding device 24 may be arranged to transfer impregnated material from the impregnation chamber 21 to the pretreatment reactor 22.
  • This feeding device 24 may also be a screw, such as a plug screw.
  • a device 27 for controlling the supply of steam to the pretreatment reactor 22 may be arranged at the pretreatment reactor 22.
  • the pretreatment reactor 22 or the feeding device 24 may thus be provided with a steam inlet.
  • the device 27 preferably comprises a valve.
  • the device 27 may for example be connected to a heating arrangement 28 for controlling the temperature of the heat supplied to the pretreatment reactor 22.
  • An emptying arrangement 25 for controlling the residence time of the cellulosic material in the pretreatment process may be arranged at the outlet of the pretreatment arrangement 2, e.g. at the outlet of the pretreatment reactor 22.
  • the emptying arrangement 25 may open the pretreatment reactor 22 such that the temperature and pressure is decreased and the pretreatment reaction is more or less terminated,
  • the emptying arrangement 25 may open the pretreatment reactor 22 to a flashing chamber (not shown) for which steam may be recovered.
  • the bioconversion arrangement 3 comprises a hydrolysis unit 31 and a fermenter 32.
  • a device 10 such as a valve, may be arranged to control the supply of pretreated slurry to the hydrolysis unit 31 .
  • Another valve 33 or a similar device may be provided at an outlet of the hydrolysis unit 31 to control the residence time of the slurry in the hydrolysis unit 31 .
  • the same or another valve (not shown) may control the supply of hydrolyzate to the fermenter 32.
  • the hydrolysis in the hydrolysis unit 31 may be acidic or enzymatic. If it is acidic, the hydrolysis unit 31 may be provided with inlet(s) for steam and/or catalyst. In such case, a device (e.g.
  • a vessel, not shown) for pH adjustment is normally arranged in the connection between the hydrolysis unit 31 and the fermenter 32.
  • a device 35 for controlling the supply of enzymes a device 36 for controlling the supply of one or more detoxification agents and/or a device 37 for controlling the supply water may be arranged at the hydrolysis unit 31 .
  • a device 38 for controlling the supply of yeast a device 39 for controlling the supply of one or more detoxification agents
  • a device 40 for controlling the supply of one or more antibacterial agents and/or a device 41 for controlling the supply water may be arranged at the fermenter 32.
  • the devices 35, 36, 37, 38, 39, 40, 41 may for example comprise valves.
  • a valve 34 or a similar device may be provided at an outlet of the fermenter 34 to control the residence time of the
  • the fermentation broth from the fermenter 32 may then, optionally after removal of insoluble matter (e.g. lignin), be transferred to a separation arrangement 1 1 , e.g. a distillation arrangement, which separates the fermentation broth into a stream enriched in the target chemical (outlet 13) and one or more stillage streams (outlet 12). If not done before, the insoluble matter may be separated from the stillage stream(s).
  • a separation arrangement 1 1 e.g. a distillation arrangement
  • a probe 4 of a NIR spectroscopy instrument is arranged to analyze the slurry from the pretreatment arrangement 2.
  • the probe may for example be arranged in connection to a slurry sample outlet 5 provided on the connection between the pretreatment arrangement 2 and the bioconversion arrangement 3.
  • the NIR analysis may be performed on a slurry sample diverted from the main piping connecting the pretreatment arrangement 2 and the bioconversion arrangement 3.
  • At least one probe 6, 8 is also arranged to analyze the slurry in the bioconversion arrangement 3.
  • a probe 6 may be arranged to analyze the slurry in the hydrolysis unit 31 and another probe 8 may be arranged to analyze the slurry in the fermenter 32.
  • the probe 6 may be arranged in connection to a slurry sample outlet 7 provided on the hydrolysis unit 31.
  • the slurry sample outlet 7 may be connected to a slurry sample inlet on the hydrolysis unit 31 such that a sampling circuit is provided.
  • the probe 8 may be arranged in connection to a slurry sample outlet 9 provided on the fermenter 31 , and the slurry sample outlet 9 may be connected to a slurry sample inlet on the fermenter 32 such that a sampling circuit is provided.
  • a probe 14 may also be arranged to analyze the cellulosic starting material supplied to the pretreatment arrangement 2. Accordingly, such a probe 14 may be arranged in an arrangement for transport of the cellulosic starting material to the pretreatment arrangement 2.
  • a single probe constitutes the probe 4 for analysis of the slurry from the pretreatment and the probe 6 for analysis of the slurry in the hydrolysis unit 31 and/or the probe 8 for analysis of the slurry in the fermenter 32.
  • the outlet 5 and the outlet 7 and/or the outlet 9 are connected to the single probe.
  • the above probe or probes 4, 6, 8, 14 may be connected to one spectrometer (not shown) each. Alternatively, two or more of the probes may be connected to a common spectrometer (not shown).
  • the probe(s) may for example be connected to the spectrometer(s) by optic fibers, The
  • spectrometer(s) is/are in turn connected to a control device 16, e.g. a computer, via signal lines 15 or a wireless communication system.
  • the control device 16 processes the data from the spectrometer(s).
  • the control device may for example comprise a screen visualizing the processed data and allowing an operator to take appropriate actions in response to them.
  • the control device 16 may automatically, i.e. without the involvement of an operator, control some parameters of the process in response to the processed data.
  • the control device 16 may for example control the feed of cellulosic starting material to the pretreatment arrangement by sending control signals to the feeding arrangement 23.
  • the feeding arrangement 23 may be connected to the control device 16 via a signal line (not shown) or a wireless communication system.
  • the control device 16 may control other parameters of the process by sending control signals to the feeding
  • the emptying arrangement 25 the device (e.g. valve) 26, the device (e.g. valve 27), the heating arrangement 28, the device (e.g. valve) 10, the device (e.g. valve) 33, the device (e.g. valve) 34, the device (e.g. valve) 35, the device (e.g. valve) 36, the device (e.g. valve) 37, the device (e.g. valve) 38, the device (e.g. valve) 39, the device (e.g. valve) 40 and/or the device (e.g. valve) 41 .
  • These recipients of control signals may also be connected to the control device via signal lines (not shown) or a wireless communication system.
  • the process conditions may be efficiently controlled.
  • the system 1 comprises a pretreatment arrangement 2 and bioconversion arrangement 3.
  • An outlet of the pretreatment arrangement 2 is connected to an inlet of the bioconversion arrangement 3, preferably via a pipe, such that slurry from the pretreatment may be supplied to the bioconversion arrangement.
  • the pH of the slurry from the pretreatment may have to be adjusted, in particular if a catalyst was added in the pretreatment (see below).
  • a device e.g. vessel, not shown
  • for pH adjustment may thus be arranged on the piping between the pretreatment arrangement 2 and the bioconversion arrangement 3.
  • the pretreatment arrangement 2 is discussed above with reference to figure 7.
  • the bioconversion arrangement 3 comprises a SSF unit 50, e.g. a fermenter, for simultaneous saccharification and fermentation of the optionally pH-adjusted slurry from the pretreatment arrangement 2.
  • a device 10 such as a valve, may be arranged to control the supply of pretreated slurry to the SSF unit 50.
  • the hydrolysis in the SSF unit 50 is normally enzymatic and in such a case, a device 35 for controlling the supply of enzymes may be arranged at the SSF unit.
  • a device 38 for controlling the supply of yeast or another biologic fermenting agent may be arranged at the SSF unit 50.
  • the devices 35, 38, 39, 40, 41 may for example comprise valves.
  • a valve 34 or a similar device may be provided at an outlet of the SSF unit 50 to control the residence time of the slurry in the SSF unit 50.
  • the fermentation broth from the SSF unit 50 may then, optionally after removal of insoluble matter (e.g. lignin), be supplied to a separation
  • arrangement 1 1 e.g. a distillation arrangement, which separates the fermentation broth into a stream enriched in the target chemical (outlet 13) and one or more stillage streams (outlet 12). If not done before, the insoluble matter may be separated from the stillage stream(s).
  • a probe 4 of a NIR spectroscopy instrument is arranged to analyze the slurry from the pretreatment arrangement 2.
  • the probe may for example be arranged in connection to a slurry sample outlet 5 provided on the connection between the pretreatment arrangement 2 and the bioconversion arrangement 3.
  • the NIR analysis may be performed on a slurry sample diverted from the main piping connecting the pretreatment arrangement 2 and the bioconversion arrangement 3.
  • a probe 8 is also arranged to analyze the slurry in the bioconversion arrangement 3, which in the present case means the slurry subjected to SSF.
  • the probe 8 may be arranged in connection to a slurry sample outlet 9 provided on the SSF unit 50.
  • the slurry sample outlet 9 may be connected to a slurry sample inlet (not shown) on the SSF unit 31 such that a sampling circuit is provided.
  • a probe 14 may also be arranged to analyze the cellulosic starting material supplied to the pretreatment arrangement 2. Accordingly, such a probe 14 may be arranged at an arrangement for transport of the cellulosic starting material to the
  • a single probe constitutes the probe 4 for analysis of the slurry from the pretreatment and the probe 8 for analysis of the slurry in the SSF unit 50.
  • the outlet 5 and the outlet 9 are connected to the single probe.
  • the above probe or probes 4, 8, 14 may be connected to one spectrometer (not shown) each. Alternatively, two or more of the probes may be connected to a common spectrometer (not shown).
  • the probe(s) may for example be connected to the spectrometer(s) by optic fibers, The
  • spectrometer(s) is/are in turn connected to a control device 16, e.g. a computer, via signal lines 15 or a wireless communication system.
  • the control device 16 processes the data from the spectrometer(s).
  • the control device may for example comprise a screen visualizing the processed data and allowing an operator to take appropriate actions in response to them.
  • the control device 16 may automatically, i.e. without the involvement of an operator, control some parameters of the process in response to the processed data.
  • the control device 16 may for example control the residence time of the slurry in the SSF unit by sending control signals to the valve 34.
  • the valve 34 may be connected to the control device 16 via a signal line (not shown) or a wireless communication system.
  • the control device 16 may control other parameters of the process by sending control signals to the feeding arrangement 23, the feeding arrangement 24, the emptying
  • control signals may also be connected to the control device via signal lines (not shown) or a wireless communication system.
  • the process conditions may be efficiently controlled.

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Abstract

Cette invention concerne un procédé de production d'un agent chimique cible à partir d'une matière première cellulosique, comprenant les étapes consistant à : a) prétraiter la matière première cellulosique dans un procédé de prétraitement pour former une suspension épaisse ; b) analyser la suspension épaisse obtenue à l'étape a) par spectroscopie PIR pour obtenir au moins un spectre PIR caractérisant la suspension épaisse obtenue à l'étape a) (premier jeu de données) ; c) soumettre la suspension épaisse obtenue à l'étape a) à saccharification et fermentation séparées ou simultanées pour obtenir un bouillon de fermentation comprenant l'agent chimique cible ; d) analyser la suspension épaisse dans une étape de l'étape c) (second jeu de données) ; et e) régler au moins un paramètre de procédé dudit procédé de prétraitement et/ou dudit procédé de saccharification et de fermentation en fonction du premier et du second jeux de données.
PCT/EP2011/070264 2010-11-17 2011-11-16 Mesures dans le pir dans la production d'un agent chimique cible à partir de cellulose WO2012066042A1 (fr)

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US9580763B2 (en) 2013-01-23 2017-02-28 Sekab E-Technology Ab Image analysis based process control of processes for production of sugar from lignocellulosic biomass
EP2759597A1 (fr) * 2013-01-23 2014-07-30 Sekab E-Technology AB Commande de processus reposant sur une analyse d'image de procédés de production de sucre à partir de biomasse lignocellulosique
WO2014160402A1 (fr) * 2013-03-14 2014-10-02 Mascoma Corporation Co-conversion de glucides en produits de fermentation dans une étape de fermentation unique
WO2015095255A1 (fr) * 2013-12-20 2015-06-25 Bp Corporation North America Inc. Procédé de contrôle et de commande d'un bioprocédé mettant en oeuvre une spectroscopie proche infrarouge et infrarouge moyen
US20160011103A1 (en) * 2014-07-08 2016-01-14 Sumitomo Electric Industries, Ltd. Optical measuring method and manufacturing method of the alcohol
JP2016017837A (ja) * 2014-07-08 2016-02-01 住友電気工業株式会社 光学測定方法及びアルコールの製造方法
WO2016126185A1 (fr) * 2015-02-02 2016-08-11 Sekab E-Technology Ab Contrôle du prétraitement d'un matériau de départ type bois résineux
EP3561064B1 (fr) * 2018-04-27 2024-02-14 Sekab E-Technology AB Procédé et système de fermentation microbienne
CN112041453A (zh) * 2018-04-27 2020-12-04 瑞典乙醇化工技术有限公司 用于微生物发酵的工艺和系统
US11965219B2 (en) 2018-05-17 2024-04-23 University Of Leeds Process and apparatus for reduction in microbial growth in solutions of sugars extracted from waste materials
WO2020157378A1 (fr) * 2019-01-29 2020-08-06 Upm-Kymmene Corporation Procédé et agencement pour commande à base de rétroaction dans le raffinage chimique de bois
US20220097252A1 (en) * 2019-01-29 2022-03-31 Upm-Kymmene Corporation Method and arrangement for feedback based control in chemical refining of wood
CN113365790A (zh) * 2019-01-29 2021-09-07 芬欧汇川集团 木材化学精炼中基于反馈的控制的方法和装置
EP4012039A1 (fr) * 2020-12-14 2022-06-15 Sekab E-Technology AB Procédé et système permettant d'augmenter la fermentabilité de la fermentation microbienne
WO2022128886A1 (fr) * 2020-12-14 2022-06-23 Sekab E-Technology Ab Procédé et système d'augmentation de la fermentescibilité de la fermentation microbienne

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