FIELD OF THE INVENTION

The invention concerns the general technical field of converting biomass into chemical bioproducts in industrial scale. In particular the invention con cerns the technology of maintaining appropriate quali- ty of the product that comes through various pretreat ing stages.

BACKGROUND OF THE INVENTION

The production of biomass-based chemicals may use for example wood particles as the main raw materi al. In a biomass-to-sugar process the wood particles may be subjected to various kinds of pretreatment such as washing and impregnating with water and/or other liquids, and subjected to elevated temperature and pressure, in order to prepare the material for the later stages of the process.

A pretreatment process may involve soaking the wood particles in steam or hot water, then soaking them in dilute acid, and subsequently taking the acid- impregnated wood particles into a hemihydrolysis reac tor where a steam explosion reaction breaks the parti cles into reaction products such as cellulose, hemi- cellulose (so-called C5 sugar), and lignin. Mechanical conveyors such as screw feeders transfer the impreg- nated wood particles between the stages of the pre treatment process.

The quality of the product that comes out of pretreatment depends on a number of factors, such as the physical and chemical conditions in the various pretreatment stages for example. The nature and imple mentation of the pretreatment process should be such that it allows continuous running for extended peri ods, so that the quality of the product that comes out of pretreatment is and can be constantly maintained within predetermined limits.

A prior art document EP 2 759 597 A1 disclos es image analysis based process control of processes for production of sugar from lignocellulosic biomass, and a corresponding system. The method comprises steps like pretreating, saccharification, analyzing parti- cles, and controlling process parameters on the basis of analysis data.

Another prior art document WO 2017/066042 A1 discloses NIR measurements in the production of a tar get chemical from cellulose. The method comprises steps like pretreating, analyzing with NIR spectrosco py, simultaneous saccharification and fermentation, analyzing anew with NIR spectroscopy, and controlling process parameters on the basis of the NIR analysis data .

SUMMARY

According to a first aspect there is provided a method for controlling values of process parameters of a pretreatment process of wood particles. The meth- od comprises using a sampler to obtain a sample of a product flow of said pretreatment process after said wood particles have undergone steam explosion in a hemihydrolysis reactor, using a particle measurement device to measure one or more characteristics of par- tides in said sample and to produce one or more piec es of measurement information indicative of the meas ured characteristics, and using said one or more piec es of measurement information to select one or more values of one or more of said process parameters.

According to a second aspect there is provid ed a control system for controlling a pretreatment process of wood particles. The control system compris- es one or more measurement information inputs for re ceiving measurement information indicative of measured characteristics of samples of a product flow in said pretreatment process. The control system comprises one or more control information outputs for set-ting val ues for one or more process parameters of said pre treatment process, and a processing engine coupled to said measurement information inputs and said control information outputs. The processing engine is pro grammed to execute a method of the kind described above .

BRIEF DESCRIPTION OF THE DRAWINGS

The accompanying drawings, which are included to provide a further understanding of the described embodiments and constitute a part of this specifica tion, illustrate various advantageous features and ex amples of their combinations. In the drawings:

Figure 1 illustrates a chemical refining pro cess on a general level,

Figure 2 illustrates an example of process stages in pretreatment, and

Figure 3 illustrates an example of a method and an arrangement for feedback based control of pro cess parameter values.

DETAILED DESCRIPTION

Numerical attributes such as first, second, third, and so on are used in this description and the appended claims for the purpose of giving unambiguous names to concepts. They do not refer to any particular order, unless otherwise explicitly stated.

In the context of this description the term wood particles refers to a material that consists mainly of pieces of wood formed by cutting or chipping larger pieces of wood such as trees, branches, logging residues, stumps, roots, and wood waste. The size of the wood particles may vary in a wide range from a few millimetres to a few centimetres, so the wood parti cles meant here are typically larger than those meant with the term sawdust. The wood used to make wood par ticles may be debarked or it main contain bark. For a wood-to-sugar process the preferred raw material is broadleaf wood due to its relatively high inherent sugar content, but the use of other kinds of wood is not excluded. The terms wood particles, wooden wood particles, or just wood particles can be used to mean the same thing as wood particles. The term wood parti cles is used in the appended drawing because it is short .

Fig. 1 illustrates schematically how in a method and arrangement for treating wood particles the wood particles may go to pretreatment, schematically illustrated as 101. The purpose of the pretreatment

101 is to prepare the incoming wood particles for ef ficient use in the process, by removing some unwanted impurities, by compensating for some of the natural fluctuations in the characteristics of the material, and by breaking down the natural structure of the wood material. Hemicellulose (C5 sugars) can be collected from the pretreatment 101, and cellulose (or lignocel- lulosic material) can be taken further to a hydrolysis

102 to produce carbohydrates of desired kind.

Fig. 2 illustrates an example of a product flow through various stages that all belong to the pretreatment 101 of fig. 1. Washing 201 is done with water, removing some mainly inorganic impurities such as sand. Washed wood particles are taken to steam treatment 202 for the purpose of removing air from in side the wood particles and to preheat them to an ele vated temperature. Steam-treated wood particles are taken to dilute acid treatment 203 for impregnating them with a dilute acid solution. The aim of the di lute acid treatment 203 is to make the dilute acid so lution penetrate into the wood particles as evenly as possible .

The acid-impregnated wood particles are taken to hemihydrolysis at 204 where they are under elevated pressure and temperature. At the output of the hemihy drolysis 204 the wood particles undergo a steam explo sion that breaks their structure. The output stream from the hemihydrolysis and steam explosion 204 goes through steam separation (not separately shown) to mixing 205 where water is added and the resulting mass is homogenized mechanically to break up agglomerates. Solids and liquids may then be separated at 206 for feeding into later process stages.

When the effective operation of the pretreat ment process is evaluated, there are a number of as pects that need to be considered. One of them is the severity of the reaction in the hemihydrolysis and steam explosion in the stage shown as 204 in fig. 2. If the reaction is too severe, the product coming out of the reactor is too finely grained; in other words the particle size distribution of the product shows too large proportions in the smallest size bins, which makes the product more difficult to handle. Also, too severe a reaction at stage 204 may produce excessive amounts of unwanted chemical constituents like lactic acid and/or furfural, which have disadvantageous ef fects in the later stages of the process, while the yield of desired chemical constituents like C5 sugars becomes low. Towards the other extreme, if the reac tion in the hemihydrolysis and steam explosion stage is too mild, i.e. not severe enough, the product com ing out of the reactor is too coarsely grained for ef fective use in the later stages of the process, and the yield of desired chemical constituents like C5 sugars is again lower than would be possible. Another aspect to be considered is the con centration and spatial distribution of acid in the wood particles when they enter the hemihydrolysis and steam explosion stage 204. If the dilute acid solution has not fully penetrated the wood particles, its cata lyzing effect on the hemicellulose hydrolysis does not take full effect. The result of incomplete penetration of dilute acid solution to the largest wood particles can be seen as an increased shive content in the prod uct that comes out of the reactor. On the other hand too much acid entering the reactor is not good either, because too high an acid concentration has a disadvan tageous effect on the proceeding of the further, de sired reactions in the process.

Another aspect to be considered consists of the homogeneity characteristics of the product after the mixing stage 205. The mixing stage could also be called dispersing, and the apparatus used may be called a mixer or a dispergator. If the mixing is not thorough enough there may occur an excessive amount of agglomerates in the mass. On the other hand, too vig orous mixing breaks the fine structure of the material grains that would be desirable, again making the par ticle size distribution skew too much towards the smallest size bins.

Fig. 3 illustrates principles of a method for controlling values of a number of process parameters. The method concerns in particular a pretreatment pro cess of wood particles, when the pretreatment is used as a preparatory stage in a wood-to-sugar process. The process comprises the pretreatment described here, be fore hydrolysis of the fraction comprising cellulose to carbohydrates (including C6 sugars) and further a catalyctic conversion of the C6 sugars to glycols, meaning ethylene glycol and propylene glycol. A pro cess parameter is a controllable quantity, like a pressure, a temperature, an acid concentration, a ro- tation rate, a residence time, a force, or the like. Controlling the value of such a process parameter may involve attempting to maintain the value at or close to a target value; or changing the value towards a new target value; or maintaining the value within a range of allowed values; or keeping the value out of a range of disallowed values; or making the value change con tinuously or periodically or repeatedly according to a control curve; or otherwise ensuring that the value is not arbitrary but a result of deliberate action.

The method comprises using a sampler to ob tain a sample of a product flow of the pretreatment process after the wood particles have undergone steam explosion in a hemihydrolysis reactor. Strictly speak ing it may be said that the steam explosion only takes place when the wood particles exit the hemihydrolysis reactor, but for the purposes of this text the output may be considered a part of the reactor. Comparing the schematic illustration in fig. 2 the sample may be ob tained between stages 204 and 205; or between stages 205 and 206; or after stage 206. The method comprises also using a particle measurement device to measure one or more characteristics of particles in the sam ple. The particle measurement device produces one or more pieces of measurement information indicative of the measured characteristics. The method comprises us ing said one or more pieces of measurement information to select one or more values of one or more of the process parameters, as will be explained in more de tail later. Selecting a value for a process parameter may mean that a value is maintained as it is (i.e. de liberately selecting the current value also for future use) or selecting a new value, so that the value of the process parameter will be changed towards the new, selected value.

As shown on the left in fig. 3, one process parameter for which a value can be selected is a tern- perature 302 in the hemihydrolysis reactor 301. Anoth er process parameter for which a value can be selected is a pressure difference 303 between an input and an output of the hemihydrolysis reactor 301. Yet another process parameter for which a value can be selected is a residence time 304 of the product flow in the hemi hydrolysis reactor 301. This residence time 304 is called here the first residence time to make a differ ence to other residence times that will be discussed later in this text.

The particle measurement device may be con figured to measure particle size or particle size dis tribution 311 in the sample. Thus the particle size - or particle size distribution - is an example of a characteristic of particles that can be measured. In a measurement of this kind measuring a particle size re fers to producing a piece of measurement information that indicates a characteristic particle size, like a size or size range that - with appropriate weighting - is a good general descriptor of a predominant particle size that has an important effect on how the mass be haves and how it can be handled. Correspondingly meas uring a particle distribution refers to producing one or more pieces of measurement information that indi cate two or more characteristic particle sizes and their relative proportions in the sample, so that the produced pieces of measurement information describe predominant particle size categories or particle size bins, occupants of which have an important effect on how the mass behaves and how it can be handled.

A particle measurement device that can be used to measure particle size and/or particle size distribution is preferably an automatic measurement device, or a device at least part of the operation of which can be automated. Optical methods are a prefera ble choice of measurement methods that can be automat ed and that produce information about particle size and/or particle size distribution. Optical measurement methods can be used to directly measure the amount and size of particles in a sample, where direct measure ment means that the optical measurement device direct ly observes the particles in question, for example by diluting the sample into a slurry and obtaining a dig ital image of the sample, to be directed to programma ble processing. Particle measurement devices that are known at the time of writing this description and that can be used this way include - but are not limited to - the Valmet FS5 fiber image analyzer and the Valmet MAP pulp analyzer.

The measured particle size or particle size distribution can be compared to a default size or a default size distribution respectively. The comparison may produce one of the pieces of measurement infor mation referred to above. In particular, the compari son may indicate larger than default particles in the sample, or smaller than default particles in the sam ple .

If the measured particle size is too large, the reaction in the hemihydrolysis reactor 301 is probably not severe enough. Correspondingly the method may comprise increasing the value of the temperature

302, the pressure difference 303, and/or the first residence time 304 in the hemihydrolysis reactor 301 to increase reaction severity in response to the pro duced piece of measurement information indicating larger than default particles in the sample. If the measured particle size is too small, the reaction in the hemihydrolysis reactor 301 is probably too severe. Correspondingly the method may comprise decreasing the value of the temperature 302, the pressure difference

303, and/or the first residence time 304 in the hemi hydrolysis reactor 301 to decrease reaction severity in response to the produced piece of measurement in- formation indicating smaller than default particles in the sample.

The temperature and pressure in the hemihy- drolysis reactor 301 have a certain connection, be cause both are basically produced by feeding saturated (typically not superheated) steam into the reactor. Increasing pressure increases also temperature, and vice versa, unless superheated steam is used. A factor that affects solely the temperature difference between the input and output of the hemihydrolysis reactor is the pressure at which the product is allowed to dis charge from the reactor.

The temperature 302 in the hemihydrolysis re actor 301 is typically between 160 and 220 degrees celcius, preferably between 185 and 205 degrees Celsi us. The pressure in the hemihydrolysis reactor is typ ically between 5.5 and 22.4 bar-g, preferably between 10.5 and 16.5 bar-g. The discharging pressure at the output of the hemihydrolysis reactor may be as high as over 3 bar-g, or in the order of magnitude of 2 bar-g, or basically down to atmospheric pressure. Controlling the pressure difference 303 between the input and out put of the hemihydrolysis reactor 301 is easiest to do by controlling the pressure inside the reactor, be cause changing the discharging pressure may require structural modifications. The first residence time 304 in the hemihydrolysis reactor 301 is typically between 2 and 20 minutes, preferably between 4 and 14 minutes.

As shown in the middle in fig. 3, one process parameter for which a value can be selected is a sec ond residence time 324 of said product flow in an im pregnating vessel that precedes said hemihydrolysis reactor in said pretreatment. This residence time is the time for which the wood particles are immersed in the dilute acid solution. Another process parameter for which a value can be selected is the acid content 323 of an impregnating solution used to impregnate said product flow in said impregnating vessel. Another process parameter for which a value can be selected is the third residence time 322 of said product flow in a first soaking silo that may precede said impregnating vessel in said pretreatment, where the wood particles are immersed in water. Such a water-impregnating stage is optional in the pretreatment process. Yet another process parameter for which a value can be selected is the fourth residence time 325 of said product flow in a pre-steaming silo that may precede said impregnating vessel (and said first soaking silo, if one is used) in said pretreatment, where the wood particles are treated with steam. Yet another process parameter for which a value can be selected is the fifth residence time of said product flow in a second soaking silo that may be used between said impregnating vessel and said hemihydrolysis reactor in said pretreatment.

The five last-mentioned process parameters all have an effect on how much acid there is within the wood particle when it enters the hemihydrolysis reactor and how evenly that acid is distributed spa tially within the wood particle. As a consequence there is certain deterministic dependency between the values of these process parameters and the shive con tent in the produce that comes out of the hemihydroly sis reactor.

The particle measurement device can be con figured to measure shive content 331 in the sample as one of the characteristics of particles that were men tioned above. Same or similar particle measurement methods and devices can be used to measure shive con tent as those used to measure particle size. Shive content is typically expressed as a percentage that should be in the order of only few percent for the shive content to be acceptable. In principle the opti mum would be no shives at all, but practice suggests that a zero shive content can only be achieved by mak- ing the reaction in the hemihydrolysis reactor so se vere that the resulting products are not usable any more to any reasonable extent later in the process.

The measured shive content can be compared to a default shive content to produce one or more of the pieces of measurement information that were referred to above. A larger value for the second residence time 324 and/or a larger value for the acid content 323 may be selected to intensify the impregnation of wood par ticles the said impregnating vessel in response to said piece of measurement information indicating larg er than default shive content. Additionally or alter natively, a larger value for the third residence time 322 or the fifth residence time mentioned above may be selected to intensify impregnation of wood particles in the first or second soaking silo respectively in response to said piece of measurement information in dicating larger than default shive content.

As was pointed out, there are upper limits beyond which it is not feasible to prolong the second residence time 324 and/or the acid content 323 of the impregnating solution. One factor that sets upper lim its may be the presence of acid residues 332 or other unwanted chemical constituents in the product that comes out of the hemihydrolysis reactor. The method may comprise using a measurement device to measure content of one or more chemical constituents in the product flow after the wood particles in the product flow have undergone steam explosion. The measurement device may produce one or more pieces of chemical con stituent information indicative of the measured con tent. The method may comprise using said one or more pieces of chemical constituent information to select one or more values of said one or more process parame ters. These chemical constituents may comprise for ex ample furfural and/or lactic acid. As shown on the right in fig. 3, one process parameter for which a value can be selected is a rota tion rate 342 of a mixer 341 that succeeds the hemihy- drolysis reactor in the pretreatment process. Another process parameter for which a value can be selected is a sixth residence time 343 of said product flow in said mixer 341. As indicated above, the mixer 341 can also be called a dispergator.

These two last-mentioned process parameters have an effect on the measured homogeneity 351 of the product. The particle measurement device may be con figured to measure homogeneity in the sample as one of the characteristics of particles. Although strictly speaking homogeneity is a property of the mass as a whole and not pertinent to any individual particle, it is nevertheless a manifestation of what kind of parti cles there are in the mass and how these particles have been treated in the preceding process stages. The measured homogeneity can be compared to a default ho mogeneity to produce one of the pieces of measurement information referred to above.

The value for the rotation rate 342 and/or the sixth residence time 343 may be increased to in tensify homogenizing of said product flow in the mixer in response to the measurement information indicating lower than default homogeneity. Lower then default ho mogeneity may mean for example a larger than default occurrence of agglomerates, which can be detected with optical methods from the sample. Too intense homoge nizing of the product flow may cause breakages in the delicate structure of the particles, which is then a possible triggering reason to decrease the rotation rate 342 and/or the sixth residence time 343. In this respect it should be noted that the particles of the product coming out of a hemihydrolysis reactor are considerably more fragile than those encountered in the production of pulp in papermaking, so that for ex ample fiber fibrillation cannot be achieved.

Homogeneity in particular, but to some extent also other features that depend on characteristics of particles, can also be measured indirectly. Thus there may be one or more of the particle measurement devices mentioned above that are configured to measure one or more characteristics of particles in the sample through an indirect measurement method that does not measure directly the presence and size of particles in the sample. An example of such a device is a particle measurement device configured to measure drainability of the sample. Drainability can be expressed in terms of dewatering time, which can be measured for example by filtration, CSF, or SF, or with an automated system like the Valmet MAP. Slower filtration means finer particles .

There are also other factors that have an ef fect on how the values for the process parameters are selected. Energy consumption 352 should be minimized in all process stages. This is one reason, in addition to the desired avoiding of breakages in particle structure, to keep the rotation rate and residence time in the mixer 341 as low as possible, although simultaneously the homogeneity 351 must be prevented from deteriorating to unacceptable levels.

Measurements results on particle size (or particle size distribution) 311, shive content 331, and homogeneity 351 may have an effect on selecting the values of also other process parameters than those that were mentioned so far. As an example, a measure ment that shows too large particle sizes may be a rea son to increase the third, fourth, or fifth residence time, the acid content in impregnation 323, and/or the second residence time 324 in the dilute acid solution.

The schematic presentation in fig. 3 can also be understood as a presentation of a control system for controlling a pretreatment process of wood parti cles. The control system comprises one or more meas urement information inputs for receiving measurement information indicative of measured characteristics of samples of a product flow in said pretreatment pro cess. In fig. 3 these are represented by the occur rence of the various measureable features in blocks 311, 331, 332, 351, and 352. The control system com prises one or more control information outputs for setting values for one or more process parameters of said pretreatment process. In fig. 3 these are repre sented by the arrows pointing to the process parameter blocks 302 to 304, 322 to 325, and 342 to 343. The control system comprises a processing engine coupled to said measurement information inputs and said con trol information outputs. As a processing engine a suitable industrial grade computer or arrangement of computers can be used. The processing engine is pro grammed to execute a method of the kind described in the foregoing.

It is obvious to a person skilled in the art that with the advancement of technology, the ideas ex plained above may be implemented in various ways. The claimed scope is thus not limited to the examples de scribed above.