Distillation boiling point

Reagents. Phenyl Azide (freshly distilled), boiling point 49-50° C., at 5 mm. The phenyl azide was prepared according to the method of Lindsay and Allen (4). 

Acetyl chloride (54 g. =075 mole) is allowed to run drop by drop from a tap funnel on to 80 g. of finely powdered anhydrous sodium acetate prepared in the manner described below. When about half of the chloride has been added the experiment is interrupted for a short time in order to stir the pasty mass of material with a bent glass rod, the lower end of which has been flattened. The rest of the acetyl chloride is then run in at such a rate that none passes over unchanged. The anhydride is now distilled from the residual salt by mean of a luminous flame kept constantly in motion. Complete conversion of the last traces of unchanged acetyl chloride to acetic anhydride is attained by adding 3 g. of finely powdered anhydrous sodium acetate to the distillate, which is finally fractionally distilled. Boiling point of acetic anhydride 138°. Yield 55-60 g. Use for acetylation, in Perkin s synthesis (Chap. V. 8, p. 232), preparation of acetophenone (Chap. IX. 3 6, p. 346). 

The nitromethane in this second distillate is separated from the water, combined with the material first obtained, thoroughly dried over calcium chloride, and then distilled. Boiling point 101°. Yield 20-24 g. (30-36 per cent of theoretical). 

The distillate from the steam distillation is twice shaken with not too much ether, and the ethereal extract, if necessary after concentration, is transferred to a wide-mouthed bottle, into which technical sodium bisulphite solution is poured in small portions with stirring (a glass rod is used) so that the aldehyde addition compound formed sets to a thick paste. The bottle is then stoppered and vigorously shaken the stopper is removed from time to time until all the benzaldehyde has entered into combination. (Odour ) The paste is now filtered with suction, and the solid on the funnel, after washing with ether, is at once decomposed by mixing it with an excess of sodium carbonate solution the liberated aldehyde is removed without delay by steam distillation. The distillate is extracted with ether, the extract is dried over a little calcium chloride, the ether is removed by distillation, and the benzaldehyde which remains is likewise distilled. Boiling point 179°. Yield 35-40 g. (70 per cent of the theoretical). 

Bran (300 g.) is stirred in a three-litre flask with a mixture of 150 c.c. of concentrated sulphuric acid and 800 c.c. of water. About 900 c.c. of the liquid are distilled and the distillate, after neutralisation with sodium carbonate, is saturated with common salt (250 g.). Of this solution 300 c.c. are again distilled and the distillate is extracted with ether after saturation with salt. The extract is dried and the ether evaporated. Then the furfural is distilled. Boiling point 162°. Yield 5-7 g. 

The enantiomeric menthols have identical physical properties (apart from their specific rotation), but the racemates differ from the optically active forms in, for example, their melting points. Although the differences between the boiling points of the stereoisomers are small, the racemates can be separated by fractional distillation. Boiling points (in °C at 101.3 kPa) are as follows ... 

To 25.5 g of NaCN at 10-20°C ware added dropwise under stirring 64 ml of glacial acetic acid and ten at 20°C a mixture of 70 ml concentrated sulfuric acid and 64 ml of glacial acetic acid. To the prepared mixture at 20-25°C was added dropwise 82 g of 2-phenyl-3-methylbutanol. The mixture was stirred at 45-50°C for 10-20 min and then at 75°C for 30 min. To the reaction mixture was added 750 ml of water. The acids was neutralized with sodium carbonate. Product was extracted with ether and distilled. Boiling point of (dimethylbenzylcarbinyl)formamide 173-176°C/0 mm, yield 63 g. 

Acetone is made from Ao-propyl alcohol by either dehydrogenation (preferred) or air oxidation. These are catalytic processes at 500°C and 40 to 50 psi. The acetone is purified by distillation, boiling point 56°C and the conversion per pass is 70 to 85 percent, with the overall yield being in excess of 90 percent. 

Excess benzene stops the reaction at the monoalkylated stage and prevents the polymerization of propylene. The cumene is separated by distillation, boiling point 153°C. Other catalysts that have been used are aluminum chloride and sulfuric acid. 

The dilute cholorohydrin solution is mixed with a 10% slurry of lime to form the oxide, which is purified by distillation, boiling point 34°C. The yield is 90 percent. 

A neural network consists of many processing elements joined together. A typical network consists of a sequence of layers with full or random connections between successive layers. A minimum of two layers is required the input buffer where data is presented and the output layer where the results are held. However, most networks also include intermediate layers called hidden layers. An example of such an ANN network is one used for the indirect determination of the Reid vapor pressure (RVP) and the distillate boiling point (BP) on the basis of 9 operating variables and the past history of their relationships to the variables of interest (Figure 2.56). 

Cryogenic distillation Boiling points Relative volatility a,j > 2 Large-scale processes Remove first freezable components... 

Increases the distillate boiling point and permits using a cheaper cooling medium. For the same cooling medium it reduces the condenser area requirements. 

Because a refinery stream spans a wide boiling range, the crude oil analysis data would be accumulated throughout that range to provide fraction properties. The intent here is to demonstrate the relationship among volume distilled, boiling point, liquid density, and sulfur content. 

Collect 5-10 mL of distillate (boiling point is around 50°C at reduced pressure). 

Figure 3. Simulated distillation boiling point curves for virgin bitumen, mal-tenes, and asphaltenes...

Figure 13.6 Simulated distillation boiling point distributions of HDPE pyrolysis condensates...

As previously described, in a heated tube held at 450 °C over a 73.8-min interval, 0.13 mol of 1,2-dimethyltetramethoxydisilane was reacted with 0.33 mol of acetylene to produce 23.1 g of liquid reaction product. Distillation of this product at atmospheric pressure yielded 11.3 g of distillate (boiling point 100-105 °C), presumably methyltrimethoxysilane (boiling point 102-103 °C). The attempted vacuum distillation of the remainder produced a polymeric mass. 

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