Processing laboratory/pilot

In close relation with industrial process, laboratory pilote equipments have been developped to test reactivity of various raw meals on samples of less than 100 kg (figure 6). 

The reactive distillation process provides an excellent example of the ever-present interaction between design and control. Both steady-state and dynamic aspects of a chemical process must be considered at all stages of the development and commercialization of a chemical process laboratory, pilot plant, and plant. 

Specific reactor characteristics depend on the particular use of the reactor as a laboratory, pilot plant, or industrial unit. AH reactors have in common selected characteristics of four basic reactor types the weH-stirred batch reactor, the semibatch reactor, the continuous-flow stirred-tank reactor, and the tubular reactor (Fig. 1). A reactor may be represented by or modeled after one or a combination of these. SuitabHity of a model depends on the extent to which the impacts of the reactions, and thermal and transport processes, are predicted for conditions outside of the database used in developing the model (1-4). 

The production of the agrochemical 6 (Scheme 5.7) is carried out batchwise via a three-step protocol. Mass balancing has been conducted for three stages of development Laboratory-, pilot- and operation scale. An LCA was available for the operation stage only. A description of this LCA including data sources and data acquisition methods was published by Geisler et al. (product A in reference [9] corresponds to product 6 here). Many parameters in the Life-Cycle Inventory (LCI) are estimated, especially utihty demands and yields of processes for the production of precursors. Uncertainty in these estimations was illustrated in a... 

The book starts with general information on fine chemicals and characteristic features of their manufacture. Tools that are used in working out new industrial processes and optimization of existing plants and processes are presented in subsequent chapters. Finally, the target of all laboratory, pilot and design activities, namely a modern production plant, is described. 

Xyloflning [Xylol refining] A process for isomerizing a petrochemical feedstock containing ethylbenzene and xylenes. The xylenes are mostly converted to the equilibrium mixture of xylenes the ethylbenzene is dealkylated to benzene and ethylene. This is a catalytic, vapor-phase process, operated at approximately 360°C. The catalyst (Encilite-1) is a ZSM-5-type zeolite in which some of the aluminum has been replaced by iron. The catalyst was developed in India in 1981, jointly by the National Chemical Laboratory and Associated Cement Companies. The process was piloted by Indian Petrochemicals Corporation in 1985 and commercialized by that company at Baroda in 1991. 

Because of the speed and high resolution of CZE separations as well as the small sample volumes required to yield information about complex protein samples, CE is increasingly being used to assess protein purity in multistep purification protocols in laboratory, pilot plant, and process scales. Similarly, it is being considered as a candidate for monitoring fermentation. 

Improvement of microbial strains for the overproduction of natural metabolites has been the hallmark of all commercial fermentation processes. Therefore, the aim of this chapter is to highlight several aspects of process improvement to yield natural products for industry at the laboratory, pilot plant and factory scales. 

Fine-chemical/custom manufacturing companies (discussed in Section 2.1) are active in process scaleup, pilot plant (trial) production, and industrial-scale exclusive and nonexclusive manufacture contract research organizations are discussed in Section 2.2, and laboratory chemical suppliers are discussed in Section 2.3. 

In the past, the scale-up was carried out by selecting best guess process parameters. The recent trend is to employ the Factorial and Modified Factorial Designs and Search Methods. These statistically designed experimental plans can generate mathematical relationships between the independent variables, such as process factors, and dependent variables, such as product properties. This approach still requires an effective laboratory/pilot scale development program and an understanding of the variables that affect the product properties. 

Figure 16 Comparison of drug release characteristics of pellets coated with an aqueous ethylcellulose dispersion using a laboratory-, pilot-, and production-scale Wurster process.

The diaphragm compressor (Fig. 4.1.35), one of the oldest leak-free process machines, is limited to lower power (< 100 kW) because sensitive metal diaphragms must be used due to the high compression temperatures and pressures. Its applications include laboratories, pilot installations, and special production facilities. An attractive feature is their very high pressure-ratio (up to 20) produced by a single stage as a result of the small dead-space and good cool-... 

The operating conditions for the three processes are very similar— only temperatures are somewhat dissimilar. The Shell Development system, employing a modified Friedel-Crafts system, operates at a lower temperature—150°-210°F vs. 250°-400°F for the other two processes. However, the equilibrium effects of the temperature differences are minimized as shown by the similarity in n-C4 and n-C5 yields shown in Table VI. Unleaded octane numbers for C5/C6 isomerate, obtained from a pure C5/C6 straight-run fraction, could not be found in the literature for the Shell process. However, pilot unit operations charging laboratory blends of n-C5, n-C6, and C6 naphthenes have been reported (26, 45). In the Shell process the use of antimony trichloride and hydrogen has considerably reduced the amount of side reactions for a Friedel-Crafts system so that the yield for this process is quite close to the yield structure for the other two processes. 

Picard V.I.Siele, "Mechanism of Formation of White Calcium Cyanamide by the Picatinny Process , PATR 2405 (1957) (Conf) 16)J.P. Picard et al, "Laboratory Pilot Plant Investigation of Picatinny Process for Producing White Calcium Cyanamide , PATR 2452 (1957) (Conf) 17)V.I.Siele et al, "Suitability of White Calcium Cyanamide for the Preparation of Guanidine Nitrate , PATR 2455 (1957) (Conf) 18)M.Blais J.P.Picard, "Effect of Various Physical Properties of Lime on the Purity of White Calcium Cyanmide Made by the Picatinny Process , PATR 2457 (1857) (Conf) 19)S. 

After the (1 x) laboratory batch is determined to be both physically and chemically stable based on accelerated, elevated temperature testing (e.g., 1 month at 45°C or 3 months at 40°C or 40°C/80% RH), the next step in the scale-up process is the preparation of the (10 x) laboratory pilot batch. The (10 x) laboratory pilot batch represents the first replicated scale-up of the designated formula. The size of the laboratory pilot batch is usually 30-100 kg, 30-100 liters, or 30,000 to 100,000 units. 

The development and application of a rigorous model for a chemically reactive system typically involves four steps (1) development of a thermodynamic model to describe the physical and chemical equilibrium (2) adoption and use of a modeling framework to describe the mass transfer and chemical reactions (3) parameterization of the mass-transfer and kinetic models based upon laboratory, pilot-plant, or commercial-plant data and (4) use of the integrated model to optimize the process and perform equipment design. 

The book describes the up-to-date fundamentals of freezedrying, not just presenting the process in all its seven steps theoretically, but explaining it with many practical examples. Many years of experience in freeze-drying allow the authors to supply valuable criteria for the selection of laboratory, pilot and production plants, discussing the advantages, drawbacks and limitations of different plant designs. 

This chapter concerns the most important reactive separation processes reactive absorption, reactive distillation, and reactive extraction. These operations combining the separation and reaction steps inside a single column are advantageous as compared to traditional unit operations. The three considered processes are similar and at the same time very different. Therefore, their common modeling basis is discussed and their peculiarities are illustrated with a number of industrially relevant case studies. The theoretical description is supported by the results of laboratory-, pilot-, and industrial-scale experimental investigations. Both steady-state and dynamic issues are treated in addition, the design of column internals is addressed. 

The simple prototype unit discussed here is capable of continuously monitoring a process stream with rapid response to surface tension changes, and accuracy within 1-2%. Initial investigations indicate that a commercial unit based on this design would be capable of data acquisition, alarm monitoring, and/or closed-loop control of a process variable in a laboratory, pilot plant or production scale installation. A commercial instrument based on the work done in this laboratory is being developed and marketed. 

Concurrent Activities. While laboratory and field evaluations are in progress, several concurrent activities including patent preparation, chemical process development, pilot plant and manufacturing estimates are involved and must be seriously addressed (10). 

The objective of scale-up in reactor design is to determine a criterion or criteria on which to base the transfer of the laboratory scale into a full-scale commercial unit. Before proceeding from a laboratory to an industrial scale, additional investigations are required. However, it is difficult to define these additional steps to gather all the information as promptly as possibe and at minimum cost. The methodology of process development leading to scale-up becomes the principal factor for the success of the operation. In achieving this purpose, experiments are classified into three main types laboratory, pilot plant, and demonstration units. 

Mobile units for photocatalytic treatment have been constructed (126,127). The European Joint Research Center laboratory pilot plant, placed on a truck, includes Ti02 loaded on membranes in UV-irradiated tubular reactors behind microfiltration and ultrafiltration modules. The waste water flow rate for this unit was typically 40 L hr-1, and hydrogen peroxide was added to the photocatalytic process (134). 

Knowing these shortcomings, the contents were grouped in sections on industrial mission statements, laboratory process development, pilots and chemical production. For the process development part of this chapter, papers were also considered with industrial coauthors, assuming that the work was (partly) done under industrial perspective and reflects fields of interest and activity of industry. 

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