Temperature correction vacuum distillation

Two heat-sensitive organic liquids of an average molecular mass of 155 kg/kmol are to be separated by vacuum distillation in a 100 mm diameter column packed with 6 mm stoneware Raschig rings. The number of theoretical plates required is 16 and it has been found that the HETP is 150 mm. If the product rate is 5 g/s at a reflux ratio of 8, calculate the pressure in the condenser so that the temperature in the still does not exceed 395 K (equivalent to a pressure of 8 kN/m2). It may be assumed that a = 800 m2/m3, /x = 0.02 mN s/m2, e = 0.72 and that the temperature changes and the correction for liquid flow may be neglected. 

The boiling point is one of the most important physical constants of a liquid. It is also easily determined with sufficient accuracy for most purposes if a reasonable quantity of a pure substance is available, for then it is only necessar to carefully distill the sample, noting both the vapor temperature and the barometric pressure. A particularly convenient apparatus for distillation of small quantities is shown in Fig. 1-10. The shape of the flask here is a desirable one because it confines the liquid to a smaller area than does a round-bottom flask. Thermometers with standard taper joints (1-in. immersion) are very convenient and reduce the possibility of contamination, and in vacuum distillation, of leakage. They are also calibrated for partial immersion, thus making emergent stem corrections (page 83) unnecessary. They... 

The barometer is an 800-mm or longer tube which is sealed at the upper end, filled with mercury (Fig. 3-la), and inserted into a pool of mercury. If it has been filled in such a way as to avoid having air trapped in the upper end (e.g., by distilling in the mercury under a good vacuum), the height of the mercury column above the pool gives the atmospheric pressure. A temperature correction is usually applied, so that the readings correspond to that of a mercury column at 0°C. The open-end manometer (Fig. 3-1/ ) is closely related to the... 

The measurement of pressure at the top of the distillation column is critical to valid distillation results because the observed vapor temperature must be corrected to the atmospheric equivalent temperature at standard pressure conditions (760mmHg). There is a general belief that the minimum pressure should be 2mmHg or greater for reasonably accurate measurements and correction to the atmospheric equivalent temperature. At pressures below 2mmHg, the pressure measurement is too inaccurate and a discontinuity can arise in the atmospheric equivalent temperature distillation curve from atmospheric to vacuum distillation. 

An introduction to the typical resin synthesis of a UF resin used as an adhesive for wood products and in industrial applications is given below. It constitutes a handy formulation for those who want to work in this field. It is not a low-formaldehyde-emission formulation. To 1000 parts by mass of 42% formaldehyde solution (methanol < 1%) are added 22% NaOH solution to pH 8.3 to 8.5,497 parts by mass of 99% urea, and the temperature raised in 50 min from ambient to 90°C while maintaining pH in the range 7.3 to 7.6 by small additions of 22% NaOH. The temperature is maintained at 90 to 91°C until the turbidity point is reached (generally another 15 to 20 min). The pH is then corrected to 4.8 to 5.1 by addition of 30% formic acid, and the temperature is raised to 98°C. The water tolerance point is reached in 18 min and the pH is then adjusted to 8.7. Vacuum distillation of the reaction water with concomitant cooling is then initiated. After distillation of the wanted amount of water to reach a resin content of 60 to 65%, the resin is cooled to 40°C, 169 parts by mass of second urea is added, the pH is adjusted to 8.5 to 8.7, and the resin is allowed to mature at 30°C for 24 to 48 h resin characteristics solids content, 60% density, 1.268 g/cm free HCHO, 0.4% viscosity, 200cP pH, 8. 

With pipe diameters of this size, the molecules do not collide with each other, but solely with the walls of equipment and tubes. Therefore, different flow laws apply here than at higher pressures where the molecules collide mostly with each other. With vapours that are sensitive to heat, the collision numbers at distillation temperatures are in the hundreds of thousands. This has a negative impact on the gentle handling of the substance to be distilled. All these factors have to be taken into account for the correct evaluation of the type and size of the vacuum pumps, the tubes and the other distillation equipment. 

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