How is chemical engineering in CBIT

Description of the research proposal

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1 Process engineering Name of the AiF Research Association (FV) File number of the FV Description of the research application 1. Research topic Steam pressure filtration - combination of water-insoluble liquid phase and steam pressure dehumidification with steam 2. Economic relevance for SMEs 2.1 Scientific, technical and economic problem in process engineering teaching and specialist literature, the description of washing and cleaning processes as well as steam pressure filtration (DDF) is largely restricted to aqueous, single-phase, i.e. H. Mixable material systems. Current investigations 1 have shown that the washing out of organic immiscible liquids from a filter cake by water can deviate significantly from the known behavior [1, 2]. Aspects such as viscosity ratios, additional capillary effects, interaction of organic solvent molecules with one another and with the solid as well as wetting properties come to the fore. There is a noticeable practical relevance for such material systems, e.g. in: cleaning after polymerization processes solvent change in multi-stage synthesis (fine chemistry) cleaning / processing after extraction processes cleaning in processing in the petroleum industry processes in environmental technology active ingredient production The DDF in multi-component systems must also be used for the Drying processes take multi-phase thermodynamics into account, which is determined by the equilibrium states in the vapor and liquid phases, temperature, pressure and the respective composition. 1 Corresponding work has been carried out at the research center as part of the IGF project BR since 2012. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 1

2.2 Economic significance of the desired research results for SMEs The DDF is a complex technology that is mainly implemented by medium-sized plant manufacturers. Since the first commercialization in the 1990s for inorganic particle systems in fine chemistry and processing technology [3], more and more complex questions have arisen for the DDF, especially in the fields of pharmaceutical, chemical and petroleum industry [4]. The current challenges lie beyond the published scientific state of knowledge, especially with regard to the influence of complex material properties on the process. 3. Scientific and technical approach 3.1 State of research and development Steam pressure filtration Steam pressure filtration (DDF) is a gas differential pressure dehumidification (GDE) in which slightly superheated or saturated steam is used instead of compressed air [5-8]. The cake formation phase does not differ from the cake formation in other filtration processes and can be described by VDI guideline 2762. Fig. 1 Schematic representation of the dehumidification process during steam pressure filtration (DDF), the conventional filtration (GDE) is shown in dashed lines for comparison. In the phase of steam application directly following the cake formation (time = 0 in Fig. 1), the local condensation of the steam in the pile pores prevents uneven mechanical displacement, the so-called flat displacement front arises. This micro-process is the main advantage of the DDF, as it allows the gas breakthrough to occur at a significantly lower saturation level than with the GDE (Figure 1). The mechanical displacement of the mother liquid is more effective with the DDF, the pile saturation after mechanical dehumidification is around 10% - as of: 07/09/16 long version of the research proposal for steam pressure filtration - Prof. Peuker page 2

3 points below that of GDE 2. Another advantage of steam pressure filtration is the use of the latent heat introduced into the pile by the steam or of the effects of mixed-phase thermodynamics (Fig. 2). Volatile components of the mother liquor can evaporate during the steam treatment, whereby the debris can be cleaned [9]. The condensate of the steam can reduce the contamination in a certain process window by means of displacement washing. The amount of condensate that arises results from the enthalpy balance. Steam only condenses as long as the temperature in the filter cake is below the local boiling point, i.e. H. as long as solid particles and residual moisture have to be heated up. The typical steam consumption depends on material properties and dehumidification behavior and thus on capillary and process pressure and is in the kg / t solids range [6]. Fig. 2 Enthalpy at the condensation front in the filter cake - transfer of latent heat from water vapor to sensible heat from the pile. The sensible heat introduced can be used in a drying phase to further reduce the residual moisture. If compressed air flows through the hot filter cake, the pore liquid evaporates into the gas phase [6]. Due to the local high temperatures, the proportion of vapor in the gas phase is very high. The necessary enthalpy of evaporation is provided by the enthalpy content of the pile, which enables fast drying kinetics, which is limited by the convective removal of the resulting vapor with the pore flow. In the course of drying, the drying speed also decreases with the temperature. Filtration with steam has been continuously researched since the late 1950s (overview of sources in [8]), but was not able to achieve its breakthrough for continuous processes until the market penetration of hyperbaric filtration in the 2000s, especially in the chemical industry. Partial aspects of the DDF such as steaming a filter cake to remove volatile components are 2 This saturation difference is product-specific. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 3

4 procedures introduced in discontinuous production processes in fine chemical and pharmaceutical production. The integrated, hybrid process management, which converts a solvent-containing suspension directly and efficiently mechanically and thermally into a slightly water-moist particle system, is not established. Apparatus that implement a DDF use higher quality construction materials such as higher alloyed steels. There are also higher demands on the thermal and mechanical load-bearing capacity of the filter media. In the case of soluble materials, crystallization effects also occur in the lines. Filter cake washing The aim of washing is to replace the liquid in the pores of a filter cake with a pure washing liquid as completely as possible. This is relevant when substances are dissolved in the pore fluid or the pore fluid itself is a contamination of the solid. After washing, only the pure washing liquid remains on the solid particles, which can be removed by drying. A significantly purer solid is obtained. If the dissolved component is not an interfering substance but the actual product of value, the washing enables the almost complete separation of the solid and the dissolved substance and thus an increased yield. Washing is primarily referred to as through-flow washing. A washing effect can also be achieved through multi-stage batch washing, also known as dilution washing, in which the moist filter cake is mashed again after a solid-liquid separation step [10]. Washing processes are usually characterized in a so-called washing curve (Figure 3, left). This shows the quality of a wash, defined by the load X, as a function of the dimensionless wash ratio (ratio of washing liquid and pore liquid). The course of a washing curve can be divided into two [11] or three [12] areas. In the first washing area, which is referred to as the displacement area, the mother liquid or pore liquid in the cake is displaced by the washing liquid in a piston-shaped flow (convective material transport). The wash filtrate therefore consists exclusively of mother liquor. The beginning of the second washing area, the transition area, is characterized by the detection of washing liquid in the washing filtrate. A mixture of mother and washing liquid flows out of the cake, since larger pores are already flowed through by pure washing liquid [13]. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 4

5 Fig. 3 Left: Schematic representation of a washing curve for loading X in the cake with and without adsorption as a function of a washing ratio; right: Scheme of the film model according to Kuo [14]. In the third area of ​​the washing curve, the diffusion area, all capillaries accessible to the washing liquid are free of mechanically displaceable mother liquid. Impurities are transported by diffusion processes from stagnant areas of the cake into the washing liquid flow. As a result, only minor changes in concentration can be observed [15]. If there is a strong adsorption of the contamination of the mother liquid on the particle surface, a constant residual load occurs within the cake, which cannot be removed further by means of a simple displacement wash. A basic model of filter cake washing is the film or side channel model presented by Kuo [14, 16]. The washing liquid flows through the capillaries in the form of a piston flow, which is limited by a film of pore liquid (Fig. 3, right). The mass transport from the pore surface or from the stagnant film is driven by the concentration gradient between the film and the core flow. Own preparatory work. Prof. Peuker has been working in the field of mechanical liquid separation for 20 years, with a focus on mechanical-thermal processes [5-7, 17-21]. Filter cake washing In recent years, various research work at the MVAT institute has dealt with the fundamentals of filter cake washing, especially in non-aqueous systems (AIF-BR 15781: Washing with chemically different washing liquids; AIF-BR 17632: Formation of a phase boundary when washing with chemically different washing liquids ; AIF-BR 18398: Washing of heaps of porous particles). As part of an industrial project, the leaching of a bitumen-laden extractant from Status: 07/09/16 Long version of the research application for steam pressure filtration - Prof. Peuker page 5

6 investigated a sand-clay filter cake (Fig. 4), what a potential partial step of a non-aqueous oil sand extraction can be [22]. Filtrate concentration ratio c / c 0 Bitumen concentration in the filtrate in Ma. % Tol: Hep 1: 0 Tol: Hep 0:% R 75% 50% c / c0 cbit, wash filtrate R (wash filtrate) R (TG analysis filter cake) R (filter cake, mass balance wash filtrate) W according to the volume of washing fluid applied Figure 4 Washing of a real Product (Kan. Oil sand) with the target product dissolved component (bitumen) in the liquid phase (R = yield; determined using various methods) In this context, the so-called graded washing was developed, in which the composition of the washing fluid during the washing process was developed the solubility of the impurity has been adjusted so that the impurity does not precipitate. Renewed wetting The wetting behavior determines the discharge of a liquid from the pore system, both during dehumidification and during washing. The washing curve (Fig. 3) shows a breakthrough point shifted in the direction of lower washing ratios when the contact angle between the washing fluid and the solid increases from 35 to 111 (Fig. 5). This means that the proportion of the ideal displacement of the mother liquid in the washing mechanism decreases as the contact angle increases. This reduces the effectiveness of the through-flow washing. Concentration ratio in the filtrate c / c 0 in - 1 0.1 0.01 DH DH DH DH, 5 1 1.5 2 Washing ratio W m in - Figure 5 Washing curves with variation of the contact angle between the washing fluid and the solid: DH θ = 35; DH θ = 77; DH θ = 86; DH θ = 111 In order to quantify the wetting behavior, an apparatus for contact angle measurement in the liquid-liquid-solid system according to the sessile drop method is available as of: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker page 6

7 hanging and lying drops available. The liquid-liquid interfacial tension is measured using a modification of the Du-Nouy method and the spinning-drop method. Fig. 6 Left: Apparatus for determining the liquid-liquid contact angle using the sessile drop method; Right: Conversion of the apparatus for contact angle measurement with hanging drops for use in the liquid-liquid-solid system Washing and cleaning effects of vapor pressure filtration In vapor pressure filtration, a layer of pure condensate forms between the vapor phase and the mother liquid. With a typical amount of steam and porosity, a washing ratio between 0.1 and 0.4 results. This thin layer has only a low washing potential. Chloride content of gypsum in ppm, 00 0.05 0.10 spec. Steam consumption in t steam / t solid rel. Chloride content pore fluid 1 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 0.00 0.05 0.10 spec. Steam consumption in t steam / t solid Figure 7 Cleaning by washing with condensate and dehumidifying, data from [21]; left: representation as a washing curve with dehumidification (open symbols completely saturated cake); right: relative chloride concentration in the pore fluid. The concentration of the impurity (Cl - ions) in the mother liquor of the residual moisture is only reduced by approx.% For the example product FGD gypsum (Fig. 7, right), which is due to the simultaneous washing and dehumidification. Together with the improved dehumidification, there is still a reduction in the chloride load of the solid by more than an order of magnitude (Fig. 7, left). Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 7

8 The cleaning of volatile components from a filter cake by DDF can also be very effective [9]. However, some preliminary tests have also shown that even less volatile components such as dodecane (Fig. 8, left) and toluene (Fig. 8, right) can be removed from a filter cake. The rewetting of the system by the condensate of the water vapor can have a strong influence. Solvent in%, 1 0.01 isooctane dodecane saturation vapor breakthrough time in s saturation in% solvent in% mass fraction saturation toluene after washing time in s saturation in% Fig. 8 Aqueous steam pressure filtration of filter cake loaded with solvent; left: model sand - alkanes; right: chemical product - toluene; Volatile impurities (iso-octane and toluene) can be removed quickly. The (hot) steam drying phase during the DDF shows good agreement between the model calculation and the experiment for the water-moist system (Fig. 9), which is visible in the characteristics of the drying front. The temperature rise to approx. 180 C indicates that there is no longer any liquid water at this measuring point. The moisture content is reduced by the sensible warmth of the superheated steam. These approaches should be expanded accordingly for a multi-phase multi-component system. Figure 9 Modeling of through-flow drying (steam drying) Representation of the local temperature in the filter cake at the respective distance from the filter medium [6]; left: model calculation; right: Associated experiment. 3.2 Working hypothesis The overriding aim of the examined variant of the steam pressure filtration (DDF) is to free filter cakes completely, both mechanically and thermally, from the mother liquid. Here mother liquid and the condensate are as at: 07/09/16 long version research proposal steam pressure filtration - Prof. Peuker page 8

9 cannot be mixed with one another. The two liquids can therefore also have significantly different wetting properties compared to the solid. According to the current state of understanding, the determining sub-steps are: the mechanical-thermal displacement through the condensation front, the washing and possible rewetting through the condensate (condensate washing) and the selective thermal drying (evaporation) of the pore liquid in the vapor stream. In particular, the investigations in the BR project have shown that wetting effects can become so strong that the existing model concepts can no longer describe the filtration or washing process with sufficient accuracy. The technological core of the DDF is the control of the mechanisms that keep the mechanical displacement front level, at least macroscopically. This process is determined by a force equilibrium between local pressure, friction and interface forces, whereby in conventional processes the interface forces are predominantly determined only by the disperse properties of the filtered suspension. In the current question, wettability can significantly influence the interface forces as an additional influencing parameter. In the case of edge angles of over 90, the sign even changes. In centrifugal dehumidification (DDZ) [23] superimposed on steam pressure, the balance between pressure and friction forces is disturbed by additional inertial forces, so that the area of ​​existence of the flat displacement front and thus excellent mechanical dehumidification is only given over parts of the cake height. The great variation possibilities of the interface forces at liquid-liquid interfaces resp.Liquid-liquid-solid boundary lines now lead to the working hypothesis that the balance of forces on the mechanical-thermal displacement front must be described in more detail in order to ensure a reliable design of the DDF. This necessitates the need to expand the model conception of the plane mechanical displacement front, which then enables a detailed statement with regard to its expansion and self-stability. For condensate washing (see Fig. 7), a systematic distinction has not yet been made between the cleaning effects through improved dehumidification and those through the exchange of residual moisture through condensate. A link between the washing models and the dehumidification model of the DDF is also pending. The status: 07/09/16 long version research proposal steam pressure filtration - Prof. Peuker page 9

10 Movement of a flat condensate front that is not disturbed by fingering can, with regard to the mechanism, possibly be seen as a separate displacement area of ​​a washing curve. It should therefore be possible to combine the expanded model by Wilkens [2], which can describe the displacement and transition area of ​​a washing curve using a dispersion approach, with the dehumidification model of the DDF or to add it upstream of it. This enables a holistic description of the process. The drying phase of the DDF can remove volatile constituents of the mother liquor as steam continues to flow through. It could be shown for single-phase pore liquids using the example of alcohol-water mixtures that the phase equilibrium, which can be described by the mixed-phase thermodynamics, determines the drying process [9]. A complete modeling has not yet been carried out due to the complexity of the necessary numerical solution. The multiphase pore liquid, which consists of immiscible condensate and mother liquid, has one less degree of freedom due to the presence of the two liquid phases, which will simplify the modeling. It can be assumed that as long as both liquid phases are present in a volume element of the filter cake, the local temperature is defined by the sum of the partial pressures. This creates a one-to-one relationship between pressure and temperature in the pile, which makes it easy to balance the effects of evaporation. An application-oriented modeling can thus be implemented as a sub-goal. 4. Solution 4.1 Processing steps and deployment of personnel Sub-goal 1 Characterization of the material systems in terms of filtration technology Since the DDF is a complex hybrid filtration and drying process, comparative values ​​of conventional filtration processes should be provided, which serve as reference values. These include the (technical) capillary pressure curve of the gas differential pressure dehumidification, the liquid-liquid capillary pressure curve 3, the washing curve of the flow-through washing with water as well as the typical filtration parameters (rc; RM; ε; ..) from the t / v over V evaluation according to VDI The wetting properties of the particle system are set so that the organic phase (mother liquid) wets the solid better than the resulting 3 The method of liquid-liquid capillary pressure measurement is being developed in the IGF project BR to characterize two-phase flows in filter cakes. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 10

11 condensate phase. These material parameters represent a challenge for purely mechanical leaching (see Fig. 5); they also predominantly occur in use. In the reference measurements, in particular, the specific microprocesses are identified and quantified that occur superimposed in a later DDF. Objectives: Provision of characteristic filtration parameters for the classification of the material systems, benchmark conventional filtration, quantification of the microprocesses involved / interpretation aid. Sub-objective 2 Mechanical displacement and cleaning effects. Due to the self-stabilizing mechanical displacement front, the DDF is a more efficient dehumidification process than conventional gas differential pressure dehumidification. The question arises as to whether the stabilizing effects also act at a double interface between steam-condensate and condensate-mother liquor. The investigations within the scope of the project have, depending on the wetting properties, e.g. In some cases, strong finger effects have been demonstrated in multi-phase displacement washing. It would be positive for the DDF if at least the interface to the vapor phase could be stabilized. Work package 2.1 Phenomenology of the displacement phase The investigations into the front stability of real filter cakes are very complex and potentially flawed. Real effects such as local crack formation, shrinkage, heterogeneous cake formation result in large fluctuations in the experimental data, which means that a very large database is required. An alternative to this is the use of sintered bodies with a comparable pore structure 4. The cylindrical sintered body with a size of 50 × 30 mm is inserted into a Teflon ring and then clamped to the steam pressure suction filter like a cake-forming unit. The sintered body saturated with the mother liquid is equipped in 3-4 levels with 4-5 thermocouples each, so that the characteristic temperature rise of the advancing front can be detected both as a function of the movement coordinate and from the position in the measuring plane. Due to the inherent stability of the sintered body, it is also possible to observe the underside (hk = 0 mm) with a thermal imaging camera (through a special sapphire glass pane). The experiments provide information on the 4 This strategy was already used in the context of the BR project and was based on a suggestion by the committee that supported the project at the time. 5 With a VGA resolution of the camera, the pixel size is approx. Μm. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 11

12 horizontal and vertical temperature profile in the pore system. The microscopic fingering, which corresponds to an axial dispersion, can be derived from the different response behavior over time in a measuring plane. Furthermore, the temperature gradient is available in the condensate phase, the steepness of which allows statements to be made about the geometric expansion of the condensate front, which may have been mixed back. Based on the phenomenological understanding, an adaptation or expansion of the model conception of the displacement front of the DDF takes place. Work package 2.2 Quantifying the mechanical displacement / displacement washing by condensate. The investigations are carried out with the conventionally configured steam pressure suction filter on filter cake (compact particles, optional surface modification for setting the wetting behavior, rc m -2, hk mm), which is expanded by a sampling unit on the filtrate side. In this way, a washing curve can be determined from the fluid balance. The residual moisture and its composition can easily be determined gravimetrically in the two-phase system; The integral composition in the cake can be inferred from a balance of the mother liquor. In addition, the composition of the pore fluid is determined directly (analysis of the drying flow after total condensation) for selected experiments. The evaluation focuses on the shape of the washing curve and on the two characteristic points: end of the displacement range and steam breakthrough. The interpretation uses the phenomenological understanding from work package 2.1. The tests are carried out at two different pressure levels in order to evaluate the influence of the different degrees of mechanical dehumidification on the washing. For the DDF, assuming that the condensate is understood as washing liquid, a washing curve can also be displayed. In particular, the transition area is dissolved here; this extends between the displacement area (single-phase wash filtrate) and the vapor breakthrough. The transition area is the contribution of the condensate washing to the cleaning result. The steam breakthrough must be seen as the defined end of the transition area, since from here on the thermal effects begin to dominate. For volatile organic phases, the washing rate will probably even increase again after the steam breakthrough. Objectives: Clarification of the existence and the process behavior of the characteristic displacement front, quantification of the washing curve of the condensate washing, status: 07/09/16 long version research proposal steam pressure filtration - Prof. Peuker page 12

13 Sub-goal 3 Experimental determination of the thermal washing and cleaning effects. The volatility of the components involved is decisive for the thermal effects. Generally speaking, the flow-through phase of the DDF can be viewed as a variant of steam distillation. The local (vapor) pressure is the sum of the partial pressures of the individual components, with the respective partial pressure corresponding to the saturation vapor pressure of the pure component. That means, as long as both components are present, there is a constant (lower) temperature. The steam pressure filtration already specifies water as a component, so the volatility of the solvent can be assessed relative to the water. There are again three borderline cases: the organic phase is more volatile than water, water has a higher volatility than the organic phase, both have a comparable volatility in the relevant pressure range. A different profile of the process temperature in the filter cake 6 will be established for each combination of substances or properties. The volatility also determines the efficiency of the contribution made by thermal cleaning to the overall result. An extremely high volatility of the organic phase leads to a low process temperature, which allows gentle processing of the solid up to the point at which this phase has been completely removed. The question becomes more complex if the vapor pressure curves of the liquids involved have different slopes and therefore do not run parallel in the pressure range under consideration. Theoretically, the case can arise that the mother liquor is more volatile than the water vapor in the higher pressure range and less volatile near ambient pressure (e.g. water - toluene), i. H. the vapor pressure curves of the two components differ in the pressure interval under consideration. This leads to recondensation effects and an undesirable local accumulation of the components to be removed. The experiments serve as an experimental basis for process modeling (sub-goal 4). They are carried out at two different pressure levels, which enables the vapor pressure behavior to be varied. The process data acquisition provides the temperature behavior, the sampling the associated filtrate composition. The 6 The shape of the temperature profile results from the pressure profile and the slope of the two steam pressure curves. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 13

14 experiments can be interrupted at characteristic process points and analyzed ex-situ. Such process points can be defined via: the vapor breakthrough, abnormalities in the temperature profile (e.g. gradual increase), the composition of the filtrate. The majority of the experiments are carried out until the mother liquid is completely discharged 7 in order to develop a large database as a benchmark for the model calculations and for the phenomenological interpretation of the process behavior. Work package 3.1 Variation in volatility The volatility of the mother liquor is varied by choosing the organic phase. The two-phase mixture boiling temperatures of the substance combinations used are evaluated over the relevant pressure range and compared with the measurement data. The aim is to prove that the evaporation can be described using the simple mixture boiling temperatures. Furthermore, a detailed analysis of the temperature curves is carried out, paying particular attention to effects that would contradict a sharp passage of a drying or evaporation front. Particularly interesting are indications of local recondensation effects. The drying kinetics can be determined by analyzing the composition of the filtrate, since the escaping vapor stream is completely condensed. A comparison with ex-situ measurements of defined aborted tests is carried out at some support points. In the latter case, the composition of the pore fluid is analyzed across the cake height. This can be done by layer-by-layer analysis of the water content (Karl Fischer titration) or, after sample preparation, via computer tomography (few measurements). In the tomograph it is possible to differentiate between the solid phase and the two liquid phases. In this way, the drying front can also be detected. Work package 3.2 Complex material behavior Intersection of the vapor pressure curves As long as there is a multiphase liquid mixture in all volume elements of the pore space, a constant temperature profile results. Due to the different volatility, two main effects can occur with directed flow along the pressure gradient: 7 At this point, the temperature profile in the cake after the steam breakthrough corresponds to that of the single-phase steam pressure filtration. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 14

15 Delay in the drying phase, as the component, which is more volatile in the high pressure range, partially condenses out again with the expansion in the vicinity of the filter cloth. The step that determines the rate is therefore the composition of the vapor phase under ambient conditions (p = pu). In the event of a high local level of condensate, the condensate could also be mechanically displaced. The evaporation front migrates from the bottom side of the filter cake into the filter cake, since the relative volatility is significantly greater at lower pressures than at higher pressures (top of the cake). The rate-determining step is therefore the volatility of the organic phase on the top of the cake at p = pddf. The experimental program is designed in such a way that these two effects can in principle occur and are identified by evaluating the temperature profiles. Depending on the relative volatility, approaches for optimizing the process management are obtained. Objectives: Experimental description of the drying phase, taking into account the characteristic multi-phase material properties (ideal and non-ideal). Sub-goal 4 Modeling and simulation calculation of the thermal drying or evaporation phase The existing model [6, 8] for the thermal drying of the filter cake with steam and air is to be expanded to enable a quantitative prediction of the drying time and kinetics in the multi-phase system. Due to Gibbs' phase rule, the complexity of the phase distribution is not too great. At a given pressure, there is a defined composition of the gas phase. The modeling is implemented in a numerical simulation program 8 which is used for model calculations with parameter variation. Due to the spatial resolution in the numerical grid, the temperature and especially the experimentally inaccessible composition profiles are calculated. The local evaporation and recondensation flows are also available for each time element. The model calculations are verified by the experimental results (sub-goal 3). In principle, it could be that several fronts / areas move offset through the pile: e.g. an evaporation front / area at low temperatures and then a heating front that brings the filter cake to saturated steam temperature Phase behavior enables a stable numerical solution - effects of mixed phase thermodynamics do not have to be taken into account. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 15

16 brings (see work package 3.2). For an energy-efficient process, it would be extremely interesting if the (operating) parameters could be set so that only evaporation occurs, i.e. H. the process of cleaning is completed before the complete heating must take place. This would enable the thermal energy for the DDF to be reduced by more than 50%. On the basis of the parameter variation, a basic, pre-competitive optimization strategy for the evaporation phase of the DDF is to be developed. The focus here is particularly on the energy expenditure, i.e. the steam consumption. In coordination with work package 2.2 and sub-goal 5, it must also be discussed what effect an energetically optimized cleaning phase has on the residual moisture as a further product property. A holistic view is sought. Objectives: Quantitative theoretical description and modeling of the drying phase; Parameter study with the developed simulation tool. Sub-goal 5 Properties of the filter cake and the filtrate after the process. Various preliminary technical investigations have shown that emulsification effects can occur between the condensate and the immiscible mother liquor, especially since the interfacial tension is significantly reduced by the rise in temperature. The emulsion process occurs because the pile can also be viewed as a static mixer. The occurrence of these disruptive effects should be quantified. For further processing, there is also the question of what minimum residual watery moisture can be achieved.A priori, a theoretical consideration would lead to the fact that the residual aqueous moisture only depends on the process parameters (especially pressure) of the DDF, but first preliminary tests show a not yet understood influence of the immiscible phase used and its material properties. Especially at low condensation temperatures due to the material properties of the system, significantly less sensible heat is available in the filter cake for the air drying phase. Thus, an advantage of the hybrid method of DDF, which can allow up to 10% saturation reduction, would be negated. Objectives: Holistic consideration of the DDF process, consideration of secondary effects (emulsion formation) and secondary target variables (residual moisture). Sub-goal 6 Report and publication A report is drawn up in accordance with the AiF guideline and the results are published, as described in more detail in the exploitation plan. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 16

17 4.2 Working diagram year first year second year third year months month FS 1 sub-goal 1 Filtration-related characterization of the material systems 2.5 1.0 0.5 0.5 0.5 sub-goal 2 mechanical displacement and cleaning effects 9.5 AP 2.1 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.25 0.25 AP 2.2 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.25 0.25 Sub-goal 3 Superimposed thermal washing and cleaning effects. 7.0 AP 3.1 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 AP 3.2 0.5 0.5 0.5 0.5 Sub-goal 4 Modeling of the thermal drying or evaporation phase 7.0 0.5 0.5 0.5 0.5 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0, 25 0.25 0.25 0.25 0.5 0.5 0.5 0.5 Sub-goal 5 Properties of the filter cake and the filtrate after the process. 2.5 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 Sub-goal 6 Report and publication 1.5 0.25 0.25 0.5 0.5 Personnel deployment at research center 1 1 Information given in the scientific training 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1 , 0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 30.0 Dr., Dipl.-Ing. TU or similar 1 Specification with final exams. 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0, 25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 7.0 Laboratory assistant or similar 1 science Auxiliary 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0 .23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 6.9 As of: 07/09 / 16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 17

18 5. Feasibility and transfer of the results 5.1 Statements on the likely industrial implementation of the R&D results after the end of the project The planned research work should on the one hand develop the process understanding for the DDF in the application under consideration and on the other hand provide a simulation approach for the technological core. This simulation approach should enable the holistic optimization of the cleaning and dehumidifying process. With these findings, industrial companies can either evaluate the suitability and applicability of the DDF for a specific question in a technology screening or even more broadly an approximate process design, i.e. H. perform basic engineering. The work generates process engineering knowledge for use in various branches of production, most of which are characterized by SMEs. On the one hand, this concerns chemical, material technology and pharmaceutical contract manufacturers / technological service providers and, on the other hand, equipment manufacturers and engineering service providers. The results and pre-competitive process descriptions developed and documented in this research project help small and medium-sized companies to effectively assert themselves in the market with their limited human resources. The investigations should enable an improved design and conception of their process chain for this SME. The aim is to make the DDF technology for complex multi-phase systems known and manageable 9. The results are used by the equipment operators in the relevant sectors of food, renewable raw materials, chemistry, raw materials, fine chemistry and biotechnology. Aspects of the results can also be implemented by other equipment manufacturers and operators in other industries. The implementation of this generated specialist knowledge in industrial practice takes place through advanced training, publications and university teaching. As of 2016, a supraregional training academy will be set up at the research center. specifically aimed at the needs of SMEs. 9 In terms of quantitative design calculations and process experience. Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 18

19 The developed phenomenological fundamentals as well as the modeling approach can be used industrially after knowledge transfer for operational problems, for plant optimization and for the technological advancement of complex production processes. 5.2 Plan for the transfer of results to the economy The central way of communicating the results is the project accompanying committee (PA), which is made up of a large number of plant and equipment manufacturers as well as potential technology users. The PA maintains close contact with the research center and thus has a direct line to the research results. As part of the planned PA meetings, specifications for the process design should also be worked out on possible potential applications (products). The results of the individual project phases are presented in the various national committees / groups Planned specific transfer measures during the project period Measure Objective / Comment Location / Framework Period Conferences, project-accompanying committee Interim reports National specialist conferences Detailed discussion with members of the project-accompanying committee (PA) Presentation and discussion of the part - and interim results in the national specialist committees e.g. ProcessNet, GVT Scientific publication of interim results in German-language specialist press (CIT, etc.) Presentation and discussion of results to application experts Research center / central location Research center Specialist groups ProcessNet every 8-12 months annually every six months - annually every six months - annually Planned specific transfer measures after completion of the project Measure Objective / Comment Location / Framework Period Creation of a final report Dissertation on the subject of incorporation into the course content A Preparation of the research results for further education events Compilation of all results in digital form Scientific qualifications of the person responsible for the research project Inclusion of the research results in edited form in the teaching content of the TU Bergakademie Freiberg in the study programs VT, UWE and WING Transfer of the results into teaching units for further education events (e.g. planned GVT course on cleaning and quality adjustment of disperse systems; Publication in specialist journals Research Center Research Center Research Center TU Bergakademie Freiberg TU Bergakademie Freiberg / EIT RawMaterials / GVT <3 months after processing Approx. 1 year after processing> 1 year after processing Approx. 1 year after processing Status: 07/09 / 16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 19

20 courses as part of the RawMaterials Academy of the KIC EIT RawMaterials) Implementation of the results of the research project Development of implementation strategies (bilateral) of specific aspects of the research results with SMEs from the area of ​​equipment manufacturers and users Development of new / improved process design using the DDF process intensification, development of new process solutions through kmu kmu and kmu in cooperation with the research center> 2 years after processing. Development of new fields of application and customer groups by kmu 6. Implementing research center Research center 1: Head: Project manager: Technical University Bergakademie Freiberg Institute for Mechanical Process Engineering and Processing Technology (MVTAT) Agricolastraße 1 / Freiberg Prof. Dr.-Ing. Urs A. Peuker Tel .: /; Fax Prof. Dr.-Ing. Urs A. Peuker Freiberg, Prof. Dr.-Ing. Urs A. Peuker Status: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 20

21 7. Bibliography [1] M. Burisch, U.A. Peuker, The influence of wetting on washing and filtration properties, in: Filtech 2015, Cologne, [2] M. Wilkens, Flushing- Removal of organic solvents from heaps and filter cakes, in: Faculty of Mechanical Engineering, Process and Energy Technology, TU Bergakademie Freiberg, Freiberg, [3] R. Bott, T. Langeloh, Steam pressure filtration - Advanced version of the continuous pressure filtration (Hi-bar filtration), Aufziehungs-Technik / Mineral Processing, 37 (1996) [4] A. Klausener , P. Wagner, TMP / Dampfdruckfiltration, in: DPMA (Ed.), Germany, 2000, pp. 6. [5] UA Peuker, W. Stahl, Scale-up of steam pressure filtration, Chemical Engineering and Processing, 38 (1999) [6] U.A. Peuker, W. Stahl, Steam pressure filtration: Mechanical-thermal dewatering process, Drying Technology, 19 (2001) [7] U.A. Peuker, W. Stahl, Scale-up and operation of a steam pressure filter on a pilot scale, Chemie Ingenieur Technik, 73 (2001) [8] S. Gerl, Steam pressure filtration - a combined mechanical / thermal differential pressure dehumidification of filter cake, in : Faculty of Chemical Engineering, University of Karlsruhe (TH), Karlsruhe, [9] UA Peuker, Separation of organic solvents from filter cakes with steam, Filtrieren & Separieren, 17 (2003) [10] M. Wilkens, U.A. Peuker, Fundamentals and recent developments in filter cake washing, Chemie-Ingenieur-Technik, 84 (2012) [11] J. Skladzien, R. Koch, Modellierung der Filterkuchenwaschung, Chemie-Ingenieur-Technik CIT, 35 (1983) [12] J. Heuser, Filter cake washing processes with special consideration of physical-chemical influences in, Universität Karlsruhe (TH), Karlsruhe, 2003, pp [13] F. Ruslim, J. Fleischer, H. Nirschl, U. Peuker, Filter cake washing for the cleaning of soluble crystalline solid particles, Chemie Ingenieur Technik, 78 (2006) [14] MT Kuo, Filter Cake Washing Performance, Aiche Journal, 6 (1960) [15] F. Ruslim, B. Hoffner, H. Nirschel, W. Stahl, Evaluation of pathways for washing soluble solids, Chemical Engineering Research and Design, 87 (2009 ) [16] MT Kuo, E.C. Barrett, Continuous Filter Cake Washing Performance, Aiche Journal, 16 (1970) 633- &. [17] U.A. Peuker, W. Stahl, Flow-through drying of preheated beds of bulk solids drying phase during mechanical-thermal demoisturing processes, Chemie Ingenieur Technik, 74 (2002) [18] U.A. Peuker, Extension of the model concept of centrifugal drying - Consideration of mechanical / thermal drying, Chemie Ingenieur Technik, 75 (2003) [19] U.A. Peuker, Interaction of liquid movement and steam condensation during steam centrifugation, International Journal of Mineral Processing, 76 (2005) [20] U.A. Peuker, S. Courturier, M. Valat, J. Vauxelaire, Optimization of mechanicalthermal displacement by combining different effects, in: Filtech Europe, Wiesbaden, Germany, status: 07/09/16 Long version of the research proposal steam pressure filtration - Prof. Peuker page 21

22 [21] et al. Peuker, W. Stahl, R. Bott, T. Langeloh, C. Blessing, Steam-pressure filtration: an improved procedure for the processing of FGD gypsum, VGB PowerTech, 81 (2001) [22] E. Schmidt, B. Wacker , UA Peuker, The non-aqueous processing of Canadian oil sand, Chemie-Ingenieur-Technik, 86 (2014) [23] U.A. Peuker, On combined steam pressure and centrifugal dehumidification, in: Faculty of Chemical Engineering, University of Karlsruhe, Karlsruhe, as of: 07/09/16 Long version of the research proposal for steam pressure filtration - Prof. Peuker, page 22

23 Process technology Name of the AiF research association (FV) Steam pressure filtration Research topic (short form) Status: Project no .: Application no .: / FV Composition of the project-accompanying committee - Members - 1) 2) Body represented Title, name SME ( exact designation with legal form and address) 1. Members from the economy 1.1 Company BASF Personal Care Nutrition GmbH Henkelstr Düsseldorf Dr. Jörg Schwarzer BASF SE Carl-Bosch-Strasse Ludwigshafen Dr. Anke Laurenzis Bayer AG Kaiser-Wilhelm-Allee Leverkusen BHS-Sonthofen An der Eisenschmelze Sonthofen, St Andreas Damm Martin Schäfer X BOKELA Ingenieurgesellschaft Tullastrasse Karlsruhe J.K.F. GmbH Co.KG Freiburger Str Pforzheim Junker Filter GmbH Carl-Benz-Str Sinsheim Egon Ehrfeld Jörg Kübler Jürgen Junker X X

24 Process technology Name of the AiF research association (FV) Steam pressure filtration Research topic (short form) Status: Project no .: Application no .: / FV Composition of the project-accompanying committee - Members - 1) 2) Body represented Title, name SME ( exact designation with legal form and address) SiCor Engineering Partners GbR Burgunderweg Bönnigheim UVR-FIA process development-environmental protection technology Chemnitzer Str Freiberg Jürgen Oeß M. Ohmann XX 1) Members of the implementing research center (s) do not count among the members of the project-accompanying committee because they are not can accompany you yourself. 2) In the case of IGF funding and its funding variants, the definition of SMEs is based on an annual turnover of up to 125 million (including affiliated companies). The SMEs represented in the project support committee, according to this definition, are ticked. The correctness of this information at the present time has been checked. BMWi 1/2014