Distilling vessel

Destillierbarkelt, /. distillabllity. Destillier-betrieb, m. distilling plant or operation. -blase, /, distilling vessel, retort, body of a still, -brlicke, /. distillation bridge, destillieren, v.t. distill. 

Destillier-gefkss, n. distilling vessel. gUc, n. distilling vessel (of glass), -liaus, n. still-house, -helm, n. still head, -kolben, m. 

The chloride is mixed on a laboratory scale with xs Ca (powder or chips) in an Fe tube in a high-T glass distillation vessel. The Fe tube protects the glass from corrosive attack by the alkali-metal vapors. The vessel is inclined and evacuated while slowly heating to 700-800°C. The liberated Rb or Cs distills onto the cooler upper walls of the vessel and runs into integral glass ampules, which are sealed under vacuum for storage. Further purification is achieved by repeated. vacuum distillation at 300°C. Yields arc theoretical. 

Here, it is assumed that all the steam condenses in the distillation vessel. In this period, the organic phase component masses remain constant. 

Here, it is assumed that all the steam condenses in the distillation vessel. In this period, the organic phase component masses remain constant The rate of heat accumulation is balanced by the heat of condensation and the heat losses. An energy balance therefore gives... 

Preparation A mixture of phenol and formaldehyde is taken in the distillation vessel. To this hydrochloric acid or sulphuric acid or oxalic acid is added. Now the reaction mixture is heated under reflex at about 100-120°C for 2-4 hours. Water is a by-products which is distilled off at the atmospheric pressure. The resin to obtained is having the Melting point 65-75°C. 

Distillation at Atmospheric Pressure.—The simple distilling flask with side tube sloping downward (Fig. 11) serves exclusively as the distilling vessel. In general the side tube should be attached high in the case of low-boiling liquids and nearer the bulb in that of less volatile liquids. 

In today s plants the product is taken out of the reactor as the liquid mixture containing the catalyst and distillation is done in a separate distillation vessel, see Figure 8.5. 

Benzonitrile (BN) [5c] The purity of commercially available BN is 99% or more and the major impurities are water, benzoic acid, isonitriles and amines. In getting pure BN, the commercial product is dried with a mild dehydrating agent like calcium chloride, the supernatant is transferred to a distilling vessel containing P205, and then it is distilled at reduced pressure under an inert atmosphere to collect the 10-80% fraction. 

When the decomposition is completed, the vessel is heated until the material just begins to reflux, and the molten product is then allowed to cool slightly in a vigorous current of carbon dioxide. The flow of gas is reduced and the grayish crude sulfide is distilled directly into the receiver where it collects as a light-yellow solid. The arm of the distilling vessel may occasionally be cleared of solidified product by fanning with a flame. 

The united ethereal solutions, which are brown in colour, are shaken for 5 minutes with potassium carbonate, then poured off, and dried for 12 hours over anhydrous sodium sulphate. When the greater part of the ether has been evaporated at ordinary pressure on a water bath, the distillation is continued under a pressure 10—12 mms. At ordinary temperature, ether first passes over. The distilling vessel is now warmed in warm water, when a first fraction is obtained, which still contains alcohol and ether, and also some glycocoll ester and alanine ester. When the temperature of the bath has risen to 55°, the main part of the alanine ester begins to boil. The operation is discontinued when, at a bath temperature of 80°, nothing more distils over. In this way 110—125 gms. distillate are obtained, consisting for the most part of alanine ester. 

C. I. Direct Yellow 12, 24895 [2870-32-8] 4,4 -Diaminostilbene-2,2 -disulfonic acid is bis-diazotized with an aqueous solution of sodium nitrite at 5°C. Next, phenol is dissolved in water, and sodium hydroxide solution and soda are added. To this solution is added the above bis-diazotized solution. Then, more 30 % sodium hydroxide solution is added. On the following morning, the solution is heated to 70 °C, and after addition of 30 % hydrochloric acid, the dye is salted out with rock salt. The damp press cake, ethanol, soda, 30 % sodium hydroxide solution, and ethyl chloride are kept in a closed stirrer vessel for 24 h at 100 °C (5 - 5.5 bar). The mixture is then cooled to 70 °C and transferred at its own pressure to a distilling vessel, from which the ethanol is distilled. After being cooled to 80 ° C, the mixture is suction filtered and dried at 100 °C. 

Contrast this availability in the inorganic realm with the substances that are readily available from organic nature. How could chemists extract pure substances from samples of plant tissue or flesh If plant or animal matter is subjected to distillation, then, typically, a black residue remains in the distillation vessel, and liquid and gaseous substances are driven off. The distillation of different plant substances produces substances that are qualitatively similar, so... 

Looking around the large hall, Friedrich would have seen a variety of glass distillation vessels. Typically, these included three parts the material to be distilled was heated in the bottom vessel, or cucurbit, condensed in the alembic (distillation head, or Helm) on top, where it then cooled and dripped through a "beak" into a receiver (Recipient). (See the Labomnt in the center of fig. 3.) Friedrich s Laboranten had a small "separation cucurbit," for instance, which could have been used for separating silver and... 

Fractional distillation A distillation process that separates a mixture into portions of different volatilities/boiling points, which may be collected in separate receivers. A fraction is one of these separately collected distillate portions. The fractionating column is the vertical column, made of inert material such as glass or stainless steel, used to separate the different fractions from the vapours coming from the distillation vessel. 

Place the resin into a suitably sized distillation vessel and proceed to distil as in the acetate work. Drops of a blood-red oil will come over, which are carefully collected by dissolving them into alcohol. Rinse any of the oil adhering to the glassware out with alcohol and combine all of the liquid into a container. Seal and allow it to stand for several days, then decant the clear tinted extract for use. This Fixed Tincture of Antimony has powerful healing properties unrecognized by modern medicine. 

Fig. 24. Apparatus for large-scale distillation with superheated steam (for o-naphthylamine, diphenylamine, etc.) (1) inlet for superheated steam (2) distillation vessel with slow stirrer (3) coil condenser.

Fie. 40. Vacuum distillation equipment for substances which solidify easily (napnthols, phenylenediamine, etc.). The apparatus for large quantities (1000-30(X) kg.) is equipped with a stirring mechanism to prevent charrine. 1, distillation vessel 2, receiver with steam or water jacket 3, steam heated times to prevent solidification 4, trap to collect water and sublimate 5, line to pump. 

Fig. 23. (a) Laboratory apparatus for distilling with superheated steam 1, steam generator 2, water trap with vertical safety tube 3, superheater 4, distillation vessel in oil bath 5, condenser with wide tube 6, device for pushing out solid material collecting in the condenser 7, receiver for distillate 8, gas line 9, cooling water. 

A mixture of 30 g. (0.16 mole) of a-naphthoyl chloride (p. 209) [Org. Syntheses Coll. Vol. 2, 425 (1943)], 30 g. (0.19 mole) of 8-methylnaphthalene, and 100 g. of carbon disulfide is cooled in an ice bath and 30 g. (0.22 mole) of powdered aluminum chloride is added slowly in small portions. The reaction mixture is stirred for 3 hours while protected from atmospheric moisture with a calcium chloride tube. The carbon disulfide is decanted from the red-brown residue, and the residue is decomposed by the gradual addition of ice and hydrochloric acid. The resulting mixture plus the carbon disulfide layer is steam-distilled to remove unreacted -methylnaphthalene. The aqueous layer is decanted from the residue in the steam distillation vessel, and the residue is treated with dilute sodium hydroxide solution. The solid remaining is washed with water and dried. The yield of crude 2-methyl-l,T-dinaphthyl ketone is 90%. Pure ketone, m.p. 140-141°, may be obtained by several recrystallizations from ethanol including activated carbon treatment. 

A mixture of 37 g. (0.25 mole) of dry dihydroxymaleic acid (p. 121) and 92 ml. of pyridine is agitated and warmed to 50-55°. If complete solution does not take place, the mixture is filtered. The clear filtrate is placed in an apparatus for vacuum distillation using an efficient water pump, and the distillation vessel is placed in a bath at 30-35°. The distillation temperature, initially at 22°, rises to 25-27° as the pyridine is removed, and the bath temperature is raised to complete removal of the pyridine. The bath temperature is then raised to 150°, and the syrupy distillate which comes over is freed of pyridine by being allowed to stand in a vacuum desiccator over concentrated sulfuric acid. The compound crystallizes on seeding and standing overnight, and the solid is triturated with a small amount of acetone and filtered. The yield of glycolic aldehyde is 9 g., or 75%. 

Phenylmagnesium bromide is prepared in the usual manner Org, Syntheses Coll. Vol. 1, 550 (1941)] from 52 g. (0.33 mole) of bromo-benzene and 7.2 g. (0.30 gram atom) of magnesium. To the solution of the Grignard reagent in ether is added a solution of 38.8 g. (0.2 mole) of Enthrone [Org. Syntheses Coll. Vol. 1, 60 (1941)] in dry thiophene-free benzene. Excess ice and dilute hydrochloric acid are added, the ether layer is separated, and the aqueous layer is extracted with ether. The combined ethereal solutions are washed with 12% aqueous alkali solution and water. The ether is evaporated, and the residue is steam-distilled. The residue from the steam-distillation vessel is taken up in ether, and the ether is evaporated. The residual syrup is heated with a mixture of 12% aqueous sodium hydroxide and 10 g. of sodium hydrosulfite. The mixture is cooled and diluted with ether the alkaline aqueous layer is separated and discarded the ethereal layer is washed thoroughly with water and the ether is evaporated. The residual 9-phenylanthracene is reciystallized from acetic acid to give 36 g. (71%) of product, m.p. 152-153°. 

A mixture of 200 g. (1.0 mole) of phenothiazine, 306 g. (1.50 mole) of iodobenzene, 120 g. of anhydrous sodium carbonate, and 10 g. of copper powder is stirred and heated to reflux for 12 hours. The reaction mixture is steam-distilled until all steam-volatile material has been removed. The solid residue remaining in the steam-distillation vessel is separated, dried, and distilled to give 176 g. (64%) of 10-phenylphenothiazine boiling at 220-223°/ mm. and melting at 92 93°. Recrystallization from glacial acetic acid gives white prisms melting at 94.5°. 

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