Laboratory data and scale-up

The successful commetcialization ofanelectrooheinieal reaction depends upon a sufficient knowledge of the process gained at the laboratory bench and in a pilot plant. This is particularly true with a new electrochefnieil process. In general a critical amount of data wilt be required in order to  

Provide the basis for modifying an existing process to suit another feedstock or a different operating point (which may be dictated by a change in overall production needs or else by economic constraints). In such cases, a working reactor may be scaled down to a convenient laboratory pilot-plant scale. 

In some cases, a certain amount of data may be available from the literature or experience but the majority of development work will start at a small laboratory scale, in order to check existing information or to extend its scope. 

The use of a small laboratory cell for early studies is attractive for several reasons  

Few supply and disposal costs for cell components, electrolytes, reactants and products, 

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The criteria for selection of laboratory reactors include equipment cost, ease of operation, ease of data analysis, accuracy, versatility, temperature uniformity, and controllabihty, suitability for mixed phases, and scale-up feasibility. 

This involves knowledge of chemistry, by the factors distinguishing the micro-kinetics of chemical reactions and macro-kinetics used to describe the physical transport phenomena. The complexity of the chemical system and insufficient knowledge of the details requires that reactions are lumped, and kinetics expressed with the aid of empirical rate constants. Physical effects in chemical reactors are difficult to eliminate from the chemical rate processes. Non-uniformities in the velocity, and temperature profiles, with interphase, intraparticle heat, and mass transfer tend to distort the kinetic data. These make the analyses and scale-up of a reactor more difficult. Reaction rate data obtained from laboratory studies without a proper account of the physical effects can produce erroneous rate expressions. Here, chemical reactor flow models using matliematical expressions show how physical... 

Collect together all the kinetic and thermodynamic data on the desired reaction and the side reactions. It is unlikely that much useful information will be gleaned from a literature search, as little is published in the open literature on commercially attractive processes. The kinetic data required for reactor design will normally be obtained from laboratory and pilot plant studies. Values will be needed for the rate of reaction over a range of operating conditions pressure, temperature, flow-rate and catalyst concentration. The design of experimental reactors and scale-up is discussed by Rase (1977). 

The equipment is quite adequate for screening purposes. In its simplest form (i.e., a glass tube in an oven), it is a relatively low cost technique that can be assembled with standard laboratory equipment. However, the simple test set-up provides no quantitative thermal data for scale-up purposes, but only T0 values. The more advanced instruments like the SEDEX and SIKAREX, which are also isoperibolic calorimetry equipment, acquire specific thermal stability data that can be used for scale-up. Furthermore, the small autoclave tests provide gas evolution data. 

The best data to use for determining whether an incompatibility exists will obviously be from testing the actual scenarios and conditions that are identified. However, this is often not practical or possible. Small-scale tests can be performed in a laboratory that can give an indication whether a reaction is expected. However, be wary of concluding that since no reaction is seen on a small scale, no effects will be realized in an industrial facility. Heat transfer effects and scale-up issues are especially important to be careful of when extrapolating small-scale results. Differences in heat transfer, mixing and other scale-up effects can cause a significant and potentially... 

Karbstein et al. (26) pursued the question smallest size laboratory bead mill that would still deliver reliable data for scale-up. In differently sized rigs (F= 0.25-25 L), a sludge consisting of limestone (dsQ= 16 pm) and 10% aqueous Luviscol solution (mass portion of solids = 0.2) was treated. It was found that the minimum size of the mill chamber should be F= 1 L. An additional unexpected, but dramatic, result was that the validity of the process characteristics... 

Laboratory Extractors. Pilot-Scale Testing, and Scale-Up. Several laboratory units arc useful in analysis, process control, and process studies. The AKUFVE contactor incorporates a separate mixer and centrifugal separator. It is an efficient instrument for rapid and accurate measurement of partition coefficients, as well as for obtaining reaction kinetic data. Miniature mixer-settler assemblies set up as continuous, bench-scale, multistage, countercurrent, liquid-liquid contactors are particularly useful Tor the preliminary laboratory work associated with flow-sheet development and optimization because these give a known number of theoretical stages. 

A number of different types of experimental laboratory units could be used to develop design data for chemically reacting systems. Charpentier [ACS Symp. Ser., 72, 223-261 (1978)] has summarized the state of the art with respect to methods of scaling up laboratory data and has tabulated typical values of the mass-transfer coefficients, interfacial areas, and contact times to be found in various commercial gas absorbers, as well as in currently available laboratory units. 

The following example will show how design and scale-up data can be obtained by model measurements with the same material system in differently sized laboratory devices. 

Vacuum and pressure laboratory filtration assemblies are shown in Figure 11.7. Mild agitation with air sometimes may be preferable to the mechanical stirrer shown, but it is important that any agglomerates of particles be kept merely in suspension and not broken up. The test record sheet of Figure 11.8 shows the kind of data that normally are of interest. Besides measurements of filtrate and cake amounts as functions of time and pressure, it is desirable to test washing rates and efficiencies and rates of moisture removal with air blowing. Typical data of these kinds are shown in Figure 11.3. Detailed laboratory procedures are explained by Bosley (1977) and Dahlstrom and Silverblatt (1977). Test and scale-up procedures for all kinds of SLS equipment are treated in the book edited by Purchas (1977). 

Selection of the laboratory reactor type and size, and associated feed and product handling, control, and analytical schemes depends on the type of reaction, reaction time scales, and type of analytical methods required. The criteria for selection include equipment cost, ease of operation, ease of data analysis, accuracy, versatility, temperature uniformity, and controllability, suitability for mixed phases, and scale-up... 

There are few data demonstrating scale-up of the grinding-rate functions S and B from pilot- to industrial-scale mills. Weller et al. [Int. J. Mineral Processing, 22, 119-147 (1988)] ground chalcopyrite ore in pilot and plant mills and compared predicted parameters with laboratory data of Kelsall [Electrical Engg. Trans., Institution of... 

Two separate models based on Dow Advanced Continuous Simulation Language (DACSL) were used in these studies. The first model used laboratory data and parameter estimation to determine the Arrhenius constants for two desired and eight undesired reactions in a process. The second model used the Arrhenius constants, heats of reaction, different physical properties, and reactor parameters (volume, heat transfer properties, jacket control parameters, jacket inlet temperature) to simulate the effect of reaction conditions (concentration, set temperature, addition rate) on the temperature of the reaction mixture, pressure and gas flow rates in the reactor, yield, and assay of the product. The program has been successfully used in two scale-ups where the optimum safe operating conditions, effect of various possible failures, and control of possible abnormal conditions were evaluated. 

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