Process development and optimization

Vor dem Sprung in die Produktion, Chemie Produktion, December 2002 Prognoses on speed of implementation PAMIRmarket study industry s demands numbering-up risks expert opinions Clariant pigment micro-reactor production smallness not an end in itself general advantages of micro flow industrial process development and optimization share of reactions suited for micro reactors hybrid approach standardized interfaces start of industrial mass production of micro reactors unit construction kit [208],... 

In another investigation, process development and optimization studies were undertaken [67]. In the framework of a study conducted as contract research for... 

Besides applications in serial screening, the process development and optimization studies mentioned above referred to the general advantages of micro flow processing in terms of enhanced heat and mass transfer [67] (see a more detailed description in [26]). 

Table 5.4-9 gives examples of the use of reaction calorimetry in process development and optimization. 

The Lab Chip instruments/methods currently commercially available generally have less resolution and are less sensitive compared to conventional CE-SDS methods. However, the high throughput of the Lab Chip technique makes it attractive for in-process monitoring during process development. The Lab Chip method is generally used for process development activities such as clone selection, cell culture process development, and optimization of the downstream purification process. 

Surveyor is suitable for parallel process development and optimization with online sampling and integrated HPLC analysis. It employs ten reaetion vessels (working volume 15-45 mL), with individually controlled reaction temperatures from —40° to -l-150°C, with the ability to reflux. Reagent addition, reaction parameter control, sampling, and HPLC injection are controlled by built-in software. 

Perform synthetic chemical research, process development and optimization for any projects entered in... 

The chapter is organized as follows. First, to establish a common language, we define some common terms from both a pharmaceutical and an engineering perspective. Subsequently, we review model-based design and optimization as a framework for product and process development and optimization, process scale-up, and continuous improvement activities. The role of process and analytical technology (PAT) methods and principles in this framework is discussed. Finally, the main areas requiring effort are identified. 

Ultimately, the real advantage of utilizing a DOE approach during process development and optimization is that ... 

Proline-catalyzed Mannich Reaction Process Development and Optimization... 

Process development and optimization Detailed process development was conducted using synthesis of (S)-16 as model reaction [60]. The preferred reaction temperature was —78 °C lower temperatures, e.g. —90 °C, resulted in no improvement. With regard to the amount of catalyst, at least 5 mol% is required to obtain high enantioselectivity. Further increasing the amount of catalyst did not, however, result in sufficient improvement to justify use of an increased amount. From a practical standpoint the short reaction time (2 h for aromatic and a,/ -unsaturated aldehydes) in combination with a high concentration of substrate (up to 0.5 mol L ) is attractive, and results in an excellent space-time yield of up to 856 g L 1 day-1. 

Process development and optimization A disadvantage is the large excess of the ketone component usually required (although in one model reaction it was shown that stoichiometric amounts can also be used Section 6.2.1.2). In addition, a further reduction of the amount of catalyst required to 20-30 mol% would be desirable for an efficient catalytic process. 

Initial synthesis of GMC for process development and optimization studies was accomplished on a small laboratory scale with synthetic runs typically yielding 5-15 g of polymer. However, in order to test GMC on a production basis and introduce it into manufacture, scale-up of the synthesis was necessary. The control of molecular properties and composition had to be considerably better than for most commercial polymers. To this end, a pilot plant for the manufacture of GMC was designed, constructed, and used to produce kilogram quantities of polymer. The scale-up of GMC provides an excellent example of how basic chemical engineering principles are employed in microcircuit fabrication, as well as some of the challenges in synthesis, process control, and purification. The major components of the pilot plant are shown in Fig. 6. 

The numerical model described above has a significant present ability to simulate a wide range of problems in polymer processing. At the same time, it is small enough to permit easy implementation in even rather small processing facilities, and for quick familiarization by process designers. We feel such a capability would lead to a significant advance in industry capability for process development and optimization. 

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