Melt crystallization description

In this description the temperature field has been taken to be linear in the coordinate y and to be independent of the shape of the melt/crystal interface. This is a good assumption for systems with equal thermal conductivities in melt and crystal and negligible convective heat transport and latent heat release. Extensions of the model that include determination of the temperature field are discussed in the original analysis of Mullins and Sekerka (17) and in other papers (18,19). 

An optimization of all three purification steps is needed for all types of melt crystallization processes in order to make melt crystallization more economically competitive. For such an optimization, a mathematical description of the phenomena is necessary. When such a description becomes reality, a great deal of progress for the unit operation melt crystallization will be made. Research in the field continues, therefore this technique is likely to have a bright future. 

Samples were melt pressed in a vacuum laboratory hot press (Carver Press, Model C) at 160°C for 30 min. The molded films were then allowed to cool to room temperature under vacuum. A dual temperature chamber for the melt crystallization experiments consists of two large thermal chambers maintained at the melt temperature (Ti = 160°C) and the crystallization temperature (Ts = 81°C, 83°C, 86°C, 89°C, 92°C or 96°C). After 5-10 min at Ti, the copper sample cell was transferred rapidly ( 2 s) to the other chamber by means of a metal rod connected to a pneumatic device. A detailed description of the arrangement of the sample and of the two detectors used to measure WAXS and SAXS simultaneously has been provided previously [32]. Each polymer sample within the copper cell was 1.5 mm thick and 7 mm in diameter and was contained between two 25 im thick Kapton films. The actual sample temperature during crystallization (T2) and melting (Ti) was monitored by means of a thermocouple inserted into the sample cell. The crystallization temperature was usually reached 120 s after transfer without overshooting. Under isothermal conditions the fluctuations in the sample temperature are less than 0.5°C. Unless stated otherwise, all references to time are times elapsed after transferring the sample to the crystaUization chamber. 

The RIS incorporates the potential of internal rotation, and is one of the most precise descriptions of a chain that preserves its chemical structure. To describe the assemblies of polymers such as polymer solutions, blends, melts, crystals, and glasses, however, RIS is still too complex and difficult to treat. To simplify the treatment of the many chain statistics, coarse-grained model chains are often used. Typical examples are described in Figure 1.2. 

Combination of WAXS and SAXS is a very efficient way of detailed description of crystallization in blends of semicrystalbne polsmiers. Baldrian and co-workers (203,204) has studied isothermal melt crystallization of blends of low molecular weight poly(ethylene oxide) (PEO) and poly(methyl methacrylate) (PMMA) using time resolved SAXSAVAXS measurements on the ELETTRA synchrotron (205). He has reported the formation of unstable PEO lamellae of nonintegrally folded... 

In the following part of this section, we provide simple mathematical descriptions of a few common features of two-phase/two-region countercurrent devices, specifically some general considerations on equations of change, operating lines and multicomponent separation capability. Sections 8.1.2, 8.1.3, 8.1.4, 8.1.5 and 8.1.6 cover two-phase systems of gas-Uquid absorption, distillation, solvent extraction, melt crystallization and adsorption/SMB. Sections 8.1.7, 8.1.8 and 8.1.9 consider the countercurrent membrane processes of dialysis (and electrodialysis), liquid membrane separation and gas permeation. Tbe subsequent sections cover very briefly the processes in gas centrifuge and thermal diffusion. 

The second transition to be discussed is a kind of lower dimensional melting. The description of the melting of a solid as a first-order phase transition is a consequence of the discontinuous change in bulk quantities at the transition point. However, every crystal is finite, and bounded by its own surface area where the process of melting may actually be initiated If there were a layer of liquid at the surface, at temperatures below the bulk melting fransition, then there is little need to activate the melting proc-... 

The following description is taken from U.S. Patent 3,116,203. A stirred solution of 75 g of 2-amino.2 -nitrobenzophenone in 700 ml of hot concentrated hydrochloric acid was cooled to 0°C and a solution of 21.5 g of sodium nitrite in 50 ml of water was added in the course of 3 hours. The temperature of the suspension was kept at 2° to 7°C during the addition. The resulting clear solution was poured into a stirred solution of 37 g of cuprous chloride in 350 ml of hydrochloric acid 1 1. The solid which had formed after a few minutes was filtered off, washed with water and recrystallized from ethanol. Crystals of 2-chloro-2 -nitrobenzophenone melting at 76° to 79°C were obtained. 

The above description applies to the system where only the growing crystal is rotated. There is at least one other way to "stir" the melt so as to control heat flow. This is illustrated as follows ... 

In this section, we focus on diffusive mass transfer. The mathematical description of mass transfer is similar to that of heat transfer. Furthermore, heat transfer may also play a role in heterogeneous reactions such as crystal growth and melting. Heat transfer, therefore, will be discussed together with mass transfer and examples may be taken from either mass transfer or heat transfer. 

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