Requirements and drying

Weighted Average Annual Energy Requirements and Drying Efficiency for Industrial Solid Dryers— Based on Surveyed Data... 

Thurnauer FI 1960 Controls required and problems enoountered in produotion dry pressing Ceramic Fabrication Processes ed W D Kingery (New York Wiley) pp 62-70... 

Note. Secondary amines, etc. in Class (ii) can be identified by their derivatives (C) and (D) above, and by their picrates when these can be readily isolated. The preparation of derivatives (D) requires the dry amine, whereas water does not aifect that of derivatives (C). 

Pyridine. The analytical reagent grade pyridine will satisfy most requirements. If required perfectly dry, it should be refluxed over potassium or sodium hydroxide pellets or over barium monoxide, and then distilled with careful exclusion of moisture (compare Fig. 77, 47, 2). It is hygroscopic, and forms a hydrate of b.p. 94-5°. Pure pyridine has b.p. 115-5°/760 mm. 

The top of the bench should always be kept clean and dry this can easily be done if a wet and a dry rag are kept at hand. Apparatus not immediately required (a) should be kept as far as possible in a cupboard beneath the bench if it must be placed on the bench, it should be arranged in a neat and orderly manner. All apparatus should be washed immediately after use and placed in a position to drain at the first opportunity, the apparatus should be dried. It must be emphasised that as a general rule a deposit of dirt or tar is more easily removed when it is freshly formed a suitable cleaning agent can usually be found while one still remembers the nature of the material or the circumstances attending its formation. It is hardly necessary to add that sohd waste and filter papers must not be thrown into the sink, and that all operations requiring the handhng of unpleasant and noxious materials sliould be carried out in the fume cupboard ( hood ). 

The silver nitrite may be prepared as described in Section 11,50, 17. The product supplied by Johnson, Matthey and Co. Ltd., of Hatton Garden, London, E.C. 1, is satisfactory it. should be washed with absolute methyl or ethyl alcohol, followed by sodium-dried ether, and dried in an electrically-heated oven at 100 for 30 minutes (longer heating results in darkening on the surface) the substance should be kept in a vacuum desiccator until required. 

The ethyl orthoformate required in this preparation may be prepared by the action of sodium upon a mixture of chloroform and dry alcohol ... 

Pour the reaction mixture into a 1-litre round-bottomed flaak, add 250 ml. of water, fit a still head and a condenser for downward distillation (Fig. II, 13, 3, but without the thermometer). Distil the mixture until about 125 ml. of distillate (two layers) have been collected. Saturate with salt (about 30 g. are required), and separate the upper layer of cj/cZohexanone extract the aqueous layer with 25-30 ml. of ether and combine the ether extract with the cycZohexanone layer. Dry with about 6 g. of anhydrous sodium or magnesium sulphate, filter the solution into a distilling flask of suitable size to which a condenser has previously been attached. Distil oflF the ether from a water bath—a beaker containing warm water is satisfactory. Distil the residual liquid from an air bath or a wire gauze, and collect the cyclohexanone at 153-156°. The yield is 16 g. 

Mix 200 g. of adipic acid intimately with 10 g. of finely-powdered, crystallised barium hydroxide. Place the mixture in a 1-litre distilling flask, fitted with a thermometer reaching to within 5 mm. of the bottom connect the flask with a condenser and receiver. Heat the mixture gradually in an air bath (1) to 285-295° during about 90 minutes and maintain it at this temperature mitil only a small amount of dry residue remains in the flask this requires a further 2 hours. The temperature must not be allowed to rise above 300°, since at this temperature the adipic acid distils quite rapidly the best working temperature is 290°. The cycZopentanone distils slowly accompanied by a little adipic acid. Separate the ketone from the water in the distillate, and dry it with anhydrous potassium carbonate this treatment simultaneously removes the traces of adipic acid present. Finally distil from a flask of suitable size and collect the cycZopentanone at 128-131°. The yield is 92 g. 

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