Mechanical separation equipment filters

Suitable feeds to a spray dryer are solutions or pumpable pastes and slurries. Such a material is atomized in a nozzle or spray wheel, contacted with heated air or flue gas and conveyed out of the equipment with a pneumatic or mechanical type of conveyor. Collection of fines with a cyclone separator or filter is a major aspect of spray dryer operation. Typical equipment arrangements and flow patterns are shown in Figure 9.14. 

Equip a 1-litre three-necked flask with a powerful mechanical stirrer, a separatory funnel with stem extending to the bottom of the flask, and a thermometer. Cool the flask in a mixture of ice and salt. Place a solution of 95 g. of A.R. sodium nitrite in 375 ml. of water in the flask and stir. When the temperature has fallen to 0° (or slightly below) introduce slowly from the separatory funnel a mixture of 25 ml. of water, 62 5 g. (34 ml.) of concentrated sulphuric acid and 110 g. (135 ml.) of n-amyl alcohol, which has previously been cooled to 0°. The rate of addition must be controlled so that the temperature is maintained at 1° the addition takes 45-60 minutes. AUow the mixture to stand for 1 5 hours and then filter from the precipitated sodium sulphate (1). Separate the upper yellow n-amyl nitrite layer, wash it with a solution containing 1 g. of sodium bicarbonate and 12 5 g. of sodium chloride in 50 ml. of water, and dry it with 5-7 g. of anhydrous magnesium sulphate. The resulting crude n-amyl nitrite (107 g.) is satisfactory for many purposes (2). Upon distillation, it passes over largely at 104° with negligible decomposition. The b.p. under reduced pressure is 29°/40 mm. 

In a 500 ml. three-necked flask, equipped with a thermometer, mechanical stirrer and efficient reflux condenser, dissolve 16 g. of sodium hydroxide pellets in 95 ml. of hot methyl alcohol. Add 49 g. of guanidine nitrate, stir the mixture at 50-65° for 15 minutes, and then cool to about 20°. Filter oflF the separated sodium nitrate and wash with two 12 ml. portions of methyl alcohol. Return the combined filtrates to the clean reaction flask, add 69 g. of sulphanilamide (Section IX,9) and stir at 50-55° for 15 minutes. Detach the reflux condenser and, with the aid of a still-head ( knee-tube ), arrange the apparatus for distillation from an oil bath with stirring about 100 ml. of methyl alcohol are recovered. Add 12 g. of pure cycZohexanol. Raise the temperature of the oil bath to 180-190° and continue the distillation. Reaction commences with the evolution of ammonia when the uiternal temperature reaches 145°. Maintain the... 

Belt Presses Belt presses were fiiUy described in the section on filtration. The description here is intended to cover only the parts and designs that apply expression pressure by a mechanism in adchtion to the normal compression obtained from tensioning the belts and pulling them over rollers of smaller and smaller diameters. The tension on the belt produces a squeezing pressure on the filter cake proportional to the diameter of the rollers. Normally, that static pressure is calculated as P = 2T/D, where P is the pressure (psi), T is the tension on the belts (Ib/hnear in), and D is the roller diameter. This calculation results in values about one-half as great as the measured values because it ignores pressure created by drive torque and some other forces [Laros, Advances in Filtration and Separation Technology, 7 (System Approach to Separation and Filtration Process Equipment), pp. 505-510 (1993)]. 

B. Tropohne. In a 1-1., three-necked, round-bottomed flask equipped with a mechanical stirrer, addition funnel, and reflux condenser are placed 500 ml. of glacial acetic acid and then, cautiously, 100 g. of sodium hydroxide pellets. After the pellets have dissolved, 100 g. of 7,7-dichlorobicyclo[3.2.0]hept-2-en-6-one is added and the solution is maintained at reflux under nitrogen for 8 hours. Concentrated hydrochloric acid is then added until the mixture is about pH 1 approximately 125 ml. of acid is required. After the addition of 1 1. of benzene, the mixture is filtered and the solid sodium chloride is washed with three 100-ml. portions of benzene. The two phases of the filtrate are separated and the aqueous phase is transferred to a 1-1. continuous extractor (Note 8) which is stirred magnetically. The combined benzene phase is transferred to a 2-1. pot connected to the extractor and the aqueous phase is extracted for 13 hours. Following distillation of the benzene, the remaining orange liquid is distilled under reduced pressure... 

The crude ester is cooled, an equal volume of benzene is added, then the free acid is neutralized by shaking with about 250 cc. of a 10 per cent solution of sodium carbonate (Note 4). The benzene solution is poured into 1300 cc. of a saturated solution of sodium bisulfite (about 60 g. of technical sodium bisulfite per 100 cc.), contained in a wide-neck bottle equipped with an efficient stirrer, and the mixture stirred for two and a half hours. The mixture soon warms up a little and becomes semi-solid. It is filtered through a 20-cm. Buchner funnel and carefully washed, first with 200 cc. of a saturated solution of sodium bisulfite, finally with two 150-cc. portions of benzene (Notes 5 and 6). The white pearly flakes of the sodium bisulfite addition product are transferred to a 3-I. round-bottom wide-neck flask equipped with a mechanical stirrer and containing 700 cc. of water, 175 cc. of concentrated sulfuric acid, and 500 cc. of benzene. The flask is heated on a steam bath under a hood, the temperature being kept at 55°, and the mixture is stirred for thirty minutes (Note 7). The solution is then poured into a separatory funnel, the benzene separated and the water layer extracted with a 200-cc. portion of benzene. The combined benzene solution is shaken with excess of 10 per cent sodium carbonate solution to remove free acid and sulfur dioxide (Note 8). The benzene is washed with a little water and then dried over anhydrous potassium carbonate (Note 9). The benzene is distilled at ordinary pressure over a free flame from a 500-cc. Claisen flask, the solution being added from a separatory funnel as fast as the benzene distils. It is advisable to distil the ester under reduced pressure although it can be done under ordinary pressure. The fraction distilling around n8°/5mm., 130710 mm., 138715 mm., 148725 mm., 155735 mm., or... 

A. (S)-Ethyl 2-(t-Butyldimethylsilyloxy)propanoate (1). A 2-L, two-necked, round-bottomed flask equipped with a mechanical stirrer and inert gas inlet (Note 1) is charged with (S)-ethyl lactate (118 g, 1.0 mol), 500 mL of dimethylformamide (DMF), and imidazole (102 g, 1.5 mol) (Note 2). The solution is cooled in a ice bath and te/ t-butyldimethy 1 si 1 y 1 chloride (TBDMSC1) (150 g, 1.0 mol) is added in three 50-g portions, at intervals of 30 min between each addition. After the addition of the third portion, a white precipitate forms. The ice bath allowed to melt gradually overnight. After 18 hr, the reaction mixture is diluted with 300 mL of water and 500 mL of hexanes. The aqueous phase is separated and extracted with 300 mL of hexanes, and the combined hexane extracts are washed with three 50-mL portions of saturated brine, dried over MgS04, filtered, and concentrated by rotary evaporation to afford 240 g (103%) of the TBDMS ether as a colorless liquid. The product is distilled under vacuum (bp 70-78°C, 0.5 mm bath temperature 95-105°C) (Note 3) to afford 222 g (96%) of ester 1 as a colorless liquid (Notes 4, 5). 

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