Packed columns installing packings into

The analytical column pack ing was made by coating 80-100 mesh Chromosorb W with 30% by weight of W-98 Silicone Gum (Union Carbide Corporation). This was vibration packed into a 6ft x inch aluminium column. The 6ft x inch precolumn was vibration packed with commercial sodium silicofluoride (Matheson Coleman and Bell). These columns were installed in the chromatograph as shown in Fig.83. 

The column is swept continuously by a carrier gas such as helium, hydrogen, nitrogen or argon. The sample is injected into the head of the column where it is vaporized and picked up by the carrier gas. In packed columns, the injected volume is on the order of a microliter, whereas in a capillary column a flow divider (split) is installed at the head of the column and only a tiny fraction of the volume injected, about one per cent, is carried into the column. The different components migrate through the length of the column by a continuous succession of equilibria between the stationary and mobile phases. The components are held up by their attraction for the stationary phase and their vaporization temperatures. 

When low boiling ingredients such as ethylene glycol are used, a special provision in the form of a partial condenser is needed to return them to the reactor. Otherwise, not only is the balance of the reactants upset and the raw material cost of the resin increased, but also they become part of the pollutant in the waste water and incur additional water treatment costs. Usually, a vertical reflux condenser or a packed column is used as the partial condenser, which is installed between the reactor and the overhead total condenser, as shown in Figure 3. The temperature in the partial condenser is monitored and maintained to effect a fractionation between water, which is to pass through, and the glycol or other materials, which are to be condensed and returned to the reactor. If the fractionation is poor, and water vapor is also condensed and returned, the reaction is retarded and there is a loss of productivity. As the reaction proceeds toward completion, water evolution slows down, and most of the glycol has combined into the resin stmcture. The temperature in the partial condenser may then be raised to faciUtate the removal of water vapor. 

Small-diameter columns. Columns with diameter less than 1 m (3 ft) are difficult to access from inside to install and maintain the trays. Cartridge trays or an oversized diameter are often used. Either option is expensive. Cartridge trays also run into problems with sealing to the tower wall and matching tower to tray hardware [Sands, Chem. Eng., p. 86 (April 2006)]. Packing is normally a cheaper and more desirable alternative. 

Only tray-type columns were considered because of the difficulty of incorporating an effective cooling circuit into a packed column. Sieve trays (as opposed to bubble or valve-type trays) were preferred because of the ease of installing cooling coils and also their low unit cost. Details of tray selection are included in Appendix G.l. 

The monoglycerides of the raffinate (the bottom product) is shown in Figure 9 as a function of the superficial velocity of the gas phase at a phase ratio of 19. At an superficial velocity of 10 mm/s the raffinate obtained with different packings is nearly the same except for the Sulzer Packing SMV. At lower superficial velocities the wire mesh packings (Sulzer CY) provide the best yields. The experiments are made at conditions where a falling film disintegrates into drops. Therefore, it seems understandable that the efficiency of the spray column and that of the collector-distributor installations do not much differ. 

In order to prevent the local temperature rise, various contrivances have been made. For example, fluorine gas is bubbled into the bath from a sparger with a 1 / 64 to 1 /4-inch holes, or a packed column is installed in the reactor to disperse fluorine gas and to facilitate heat transfer. Neat fluorine or fluorine diluted with N2 is used for such a purpose. At around 150°C, 58% NF3 can be obtained on the basis of fluorine. 

---