Minimum agitation volume

Zinc cyanide. Solutions of the reactants are prepared by dis solving 100 g. of technical sodium cyanide (97-98 per cent. NaCN) in 125 ml. of water and 150 g. of anhydrous zinc chloride in the minimum volume of 50 per cent, alcohol (1). The sodium cyanide solution is added rapidly, with agitation, to the zinc chloride solution. The precipitated zinc cyanide is filtered off at the pump, drained well, washed with alcohol and then with ether. It is dried in a desiccator or in an air bath at 50°, and preserved in a tightly stoppered bottle. The yield is almost quantitative and the zinc cyanide has a purity of 95-98 per cent. (2). It has been stated that highly purified zinc cyanide does not react in the Adams modification of the Gattermann reaction (compare Section IV,12l). The product, prepared by the above method is, however, highly satisfactory. Commercial zinc cyanide may also be used. 

Propyl-methyl-carbinyl allyl barbituric acid (also called allyl 1-methyl-butyl barbituric acid) may be prepared as follows 1 mol of propyl-methyl-carbinyl barbituric acid is dissolved in a suitable vessel In a 10 to 35% aqueous solution of 1 mol of potassium hydroxide. To this are added somewhat in excess of 1 mol of allyl bromide, and alcohol equal to about 10% of the total volume of the solution. The vessel Is agitated for 50 to 75 hours. At the end of this time, the solution, which may still exhibit two layers, is concentrated to about one-half its volume to remove the excess allyl bromide and the alcohol. On cooling, an oily layer, which is propyl-methyl-carbinyl allyl barbituric acid, separates out as a sticky viscous mass. It is dried, washed with petroleum ether, and dissolved in the minimum amount of benzene. Any unreacted propyl-methyl-carbinyl barbituric acid, which does not dissolve, is filtered off. The addition of petroleum ether to the clear filtrate causes the propyl-methyl-carbinyl allyl barbituric acid to precipitate as an oily mass. 

Reaction occurs in the loop as well as in the stirred tank, and it is possible to eliminate the stirred tank so that the reactor volume consists of the heat exchanger and piping. This approach is used for very large reactors. In the limiting case where the loop becomes the CSTR without a separate agitated vessel, Equation (5.35) becomes q/Q > 10. This is similar to the rule-of-thumb discussed in Section 4.5.3 that a recycle loop reactor approximates a CSTR. The reader may wonder why the rule-of-thumb proposed a minimum recycle ratio of 8 in Chapter 4 but 10 here. Thumbs vary in size. More conservative designers have... 

A turbine type agitator is commonly used for liquid-solid systems. Mixing rates depend on the forces required to suspend all solid particles. Minimum levels can be determined for (1) lifting the particles, and (2) for suspending them in an homogeneous manner [200]. Similar requirements apply to liquid-liquid systems. For cases where two poorly miscible fluids of about equal volume are used in the reaction, the mixer is placed at the interface. For a bench-scale experimental system of about 2 liters capacity, the minimum rotational speed to obtain well-dispersed system is 300 to 400 rpm [201], depending on the type of mixer. This rotational value decreases as the vessel volume increases. 

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