Preparing components Preliminary operations

Reactive (chemical) molding technology and the equipment used depend on the geometrical shape of the article produced. In all cases, initial liquid products are delivered into a mold where the processes of polymerization (solidification), structure formation, and shaping proceed simultaneously. 

The preliminary operations of preparation of the initial components can be carried out in special centralized chemical production plants or directly in the work bays where the articles are manufactured. When the initial components are obtained in the form of semi-finished products, the manufacturing process is simplified. Semi-finished products are single- or, more often, two-component mixtures, especially die prepolymers used in polyurethane production. Mixtures include chemical reactants and mixtures of polymers or oligomers with different additives required for final items. 

The batch process equipment used for preparing the components is essentially a set of reactors equipped with heaters and agitators. They operate under vacuum or in an inert gas atmosphere. One of the main requirements of the chemical molding process is the production of pore- and defect-free articles. The volatile products and moisture must be thoroughly removed from the reactant mixture. Moisture imparts porosity to the final articles due to evaporation and the chemical interaction of water with the components of the reactant system, for example, with isocyanates in case of polyurethane formulations. In some cases, moisture can also inhibit the polymerization process, for example, anionic-activated polymerization of lactams. Many monomers, particularly acrylic compounds, require removal of die inhibitors to increase their shelf-life. 

If a monomer or an oligomer is delivered in heated tanks, it is immediately pumped into a heated vessel for storage in controlled conditions. Other products, which are liquid during transportation, are treated in the same way. Components with melting points higher than room 

An important step in the production process is the preparation of a standard specimen. This specimen is used to qualify principle production parameters such as the long-term stability of the reactive mixture, polymerization cycle, and the performance characteristics of the material obtained. Simultaneous determination of the reaction parameters allows us to use mathematical modelling to optimize the reactive processing regime. 

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The most convenient and economic techniques of choice for the rapid analysis of starting materials and for the assessment of purity of a crude reaction product are t.l.c. and g.l.c. These techniques may also be used to monitor the progress of a reaction for which optimum conditions are uncertain, as may be the case when an established published procedure is used as the basis for carrying out other preparations of a similar nature. In these cases the reaction is monitored by the periodic removal from the reaction mixture of test portions for suitable chromatographic study. Clearly the chromatographic behaviour of starting materials and, if possible, expected products, needs to be established prior to the commencement of the reaction. For t.l.c. this would include solvent and thin layer selection, a detection method, and an appraisal of sensitivity of detection with respect to the concentration of components in the reaction medium. For g.l.c. preliminary experiments would be required to select a suitable column and the appropriate operating conditions. 

The preparation of a derivative of a sample compound prior to GC is a significant potential source of both qualitative and, in particular, quantitative errors. Almost all reactions that are used for derivatization are organic syntheses adapted to the micro-scale. This approach makes full use of an advantageous property of GC, namely the need to take only very small amounts of the sample for the analysis, but on the other hand, it makes heavy demands on the quality of the materials used and the precision of the operating procedures. As GC has especially been used in analyses of complex mixtures with large contents of various components, such as biological samples, the operations necessary for the preliminary separation of the compounds of interest from the sample, e.g., extraction or TLC, are often involved in the entire procedure, and make it even more complicated. With some reactions, the necessity for an anhydrous medium requires the application of drying (lyophilization) in the treatment of the sample. 

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