Liquors, distilled

Within the last five years, there s been a huge trend of distillers bottling tequila on their own, instead of selling it to die larger distillers, Mr. Harrington said. The liquor, distilled from the sap of the agave plant, must be produced in Mexico to be called tequila. The state of Jalisco produces 99 percent of tequila sold. 

The alcoholic solution that results from fermentation contains only 12-15% alcohol, because yeast cells cannot survive higher concentrations. Distillation increases the alcohol concentration to about 40-50% (80 to 100 proof ) for hard liquors. Distillation of ethanol-water solutions cannot increase the ethanol concentration above 95% because a solution of 95% ethanol and 5% water boils at a lower temperature (78.15 °C) than either pure water (100 °C) or pure ethanol (78.3 °C). Such a mixture of liquids that boils at a lower temperature than either of its components is called a minimum-boiling azeotrope. 

A.—I have observed thus much, that three ounces, or a little more, of urine, taken from a healthy man, will moderately outweigh about eighty grains of fountain water, from which also I have seen a liquor distilled which was of equal weight to the said water, whence it is evident that most of the salt was left behind. 

Chem. Descrip. 6-Acetoxy-2,4-dimethyl-m-dioxane CAS 828-00-2 EINECS/ELINCS 212-579-9 Uses Antimicrobial, presenrative, bacteriostat, tungistat, preservative for industrial water-based systems and emulsions incl. paints, coatings, textile finishes, adhesives, leather processing liquors, distillate fuels Features Patented broad-spectrum wide pH range usage Regulatory EPA reg. no. 824-7... 

Tertiary butyl alcohol, trimethyl carbinol, tertiary butanol. 2-methyl-2-propanol, Me3COH. Colourless prisms, m.p. 25°C, b.p. 83°C. Prepared by absorbing isobutene (2-methylpropene) in sulphuric acid, neutralizing and steam distilling the liquor. Converted to isobutene by heating with oxalic acid. Potassium-/-buloxide is a very strong base. 

This reaction is also used on a large scale, to obtain iodine from seaweed. The ash from burnt seaweed ( kelp ) is extracted with water, concentrated, and the salts other than iodides (sulphates and chlorides) crystallise out. The more soluble iodides remain and the liquor is mixed with sulphuric acid and manganese dioxide added the evolved iodine distils off and is condensed. 

If the mother-liquor from the crude product (together with the washings) is concentrated to nearly half its original volume by gentle distillation, and is then cooled and seeded with a trace of the first crop, a second and less pure crop of the a-methylglucoside is obtained. This should be purified by recrystallisation from the mother-liquor obtained from the recrystallisation of the first crop, and then if necessary recrystallised a second time from a small quantity of fresh methanol. Yield of second crop, about... 

Sometimes an air bubble enters the tube E and prevents the regular flow of liquid from B the air bubble is easily removed by shaking the rubber tube. The flask A is heated (e.g., by a ring burner) so that distillation proceeds at a rapid rate the process is a continuous one. If the liquid to be steam distilled is lighter than water, the receiver must be modified so that the aqueous liquors are drawn off from the bottom (see Continvmia Extraction of Liquids, Section H, 44). 

Mix together in a 250 ml. flask carrying a reflux condenser and a calcium chloride drying tube 25 g. (32 ml.) of freshly-distilled acetaldehyde with a solution of 59-5 g. of dry, powdered malonic acid (Section 111,157) in 67 g. (68-5 ml.) of dry pyridine to which 0-5 ml. of piperidine has been added. Leave in an ice chest or refrigerator for 24 hours. Warm the mixture on a steam bath until the evolution of carbon dioxide ceases. Cool in ice, add 60 ml. of 1 1 sulphuric acid (by volume) and leave in the ice bath for 3-4 hours. Collect the crude crotonic acid (ca. 27 g.) which has separated by suction filtration. Extract the mother liquor with three 25 ml. portions of ether, dry the ethereal extract, and evaporate the ether the residual crude acid weighs 6 g. Recrystallise from light petroleum, b.p. 60-80° the yield of erude crotonic acid, m.p. 72°, is 20 g. 

Concentrate the mother liquors from this recrystallisation and combine with the oily filtrate dissolve in 250 ml. of 10 per cent, sodium hydroxide solution, and extract with two 50 ml. portions of ether to remove non-phenolic products. Acidify the alkaline solution with hydrochloric acid, separate the oily layer, dry it over anhydrous magnesium sulphate, and distil under diminished pressure, preferably from a Claisen flask with fractionating side arm (Figs. II, 24, 2-5). Collect the o-propiophenol (65 g.) at 110-115°/6 mm. and a further quantity (20 g.) of crude p-propiophenol at 140-150°/ 1 mm. 

Cautiously add 250 g. (136 ml.) of concentrated sulphuric acid in a thin stream and with stirring to 400 ml. of water contained in a 1 litre bolt-head or three-necked flask, and then dissolve 150 g. of sodium nitrate in the diluted acid. Cool in a bath of ice or iced water. Melt 94 g. of phenol with 20 ml. of water, and add this from a separatory funnel to the stirred mixture in the flask at such a rate that the temperature does not rise above 20°. Continue the stirring for a further 2 hours after all the phenol has been added. Pour oflF the mother liquid from the resinous mixture of nitro compounds. Melt the residue with 500 ml. of water, shake and allow the contents of the flask to settle. Pour oflF the wash liquor and repeat the washing at least two or three times to ensure the complete removal of any residual acid. Steam distil the mixture (Fig. II, 40, 1 or Fig. II, 41, 1) until no more o-nitrophenol passes over if the latter tends to solidify in the condenser, turn oflF the cooling water temporarily. Collect the distillate in cold water, filter at the pump, and drain thoroughly. Dry upon filter paper in the air. The yield of o-nitrophenol, m.p. 46° (1), is 50 g. 

Phthalide. In a 1 litre bolt-head flask stir 90 g. of a high quality zinc powder to a thick paste with a solution of 0 5 g. of crystallised copper sulphate in 20 ml. of water (this serves to activate the zinc), and then add 165 ml. of 20 per cent, sodium hydroxide solution. Cool the flask in an ice bath to 5°, stir the contents mechanically, and add 73-5 g. of phthalimide in small portions at such a rate that the temperature does not rise above 8° (about 30 minutes are required for the addition). Continue the stirring for half an hour, dilute with 200 ml. of water, warm on a water bath imtil the evolution of ammonia ceases (about 3 hours), and concentrate to a volume of about 200 ml. by distillation vmder reduced pressure (tig. 11,37, 1). Filter, and render the flltrate acid to Congo red paper with concentrated hydrochloric acid (about 75 ml. are required). Much of the phthalide separates as an oil, but, in order to complete the lactonisation of the hydroxymethylbenzoic acid, boil for an hour transfer while hot to a beaker. The oil solidifles on cooling to a hard red-brown cake. Leave overnight in an ice chest or refrigerator, and than filter at the pump. The crude phthalide contains much sodium chloride. RecrystaUise it in 10 g. portions from 750 ml. of water use the mother liquor from the first crop for the recrystaUisation of the subsequent portion. Filter each portion while hot, cool in ice below 5°, filter and wash with small quantities of ice-cold water. Dry in the air upon filter paper. The yield of phthalide (transparent plates), m.p. 72-73°, is 47 g. 

A further small quantity may be recovered from the mother liquors by removing the solvent at atmospheric pressure and distilling the residue under reduced pressure the anhydride passes over at 184-186°/ 8 mm. 

In order to control the concentration of lower dibasic acid by-products in the system, a portion of the mother liquor stream is diverted to a purge treatment process. Following removal of nitric acid by distillation (Fig. 3, K), copper and vanadium catalyst are recovered by ion-exchange treatment (Fig. 

Preparation from Waste Sulfite Liquors. The starting material for vanillin production can also be the lignin (qv) present in sulfite wastes from the ceUulose industry. The concentrated mother Hquors are treated with alkaH at elevated temperature and pressure in the presence of oxidants. The vanillin formed is separated from the by-products, particularly acetovanillone, 4-hydroxy-3-methoxyacetophenone, by extraction, distillation, and crystallization. 

In England, the Magna Carta provided a standard of measurement for the sale of ale and wine. In 1643, the English Parliament proposed the first tax on distilled spirits. In the American colonies, William Kieft, Director General of New Nethedand, imposed the first liquor tax of two guilders on each half vat of beer in 1640. Alexander Hamilton initiated an excise tax on domestic spirits in 1791. The tax was resented and ultimately repealed in 1800 by Thomas Jefferson. Except during the War of 1812, domestic spirits remained untaxed until 1862. At that time, a tax of 0.02/L was implemented, which has been increased periodically. In January 1991, the Pederal Excise Tax on distilled spirits was raised to 3.56 per titer or 13.50 per proof gallon. In addition, many states have substantially increased the state excise taxes on distilled spirits. 

There are many types, and only the most important can be mentioned here. [See also Hunter, in Dunstan (ed.). Science of Petroleum, vol. 3, Oxford, New York, 1938, pp. 1779-1797.] They are used fairly extensively in treating petroleum distillates, in vegetable-oil, refining, in extraction of phenol-bearing coke-oven liquors, in some met extractions, and the like. Kalichevsky and Kobe (Petroleum Refining... 

The united filtrate is evaporated on the steam bath until the volume amounts to 200 cc., at which point crystals should have already begun to separate from the hot solution. After standing at room temperature for twenty-four hours or longer, the crystals are filtered by suction as free from mother liquor as possible and recrystallized from an equal weight of distilled water (Note 5). The filtrate from this recrystallization is evaporated on the steam bath and the second crop of /-tartaric acid filtered and recrystallized as before. The -yield is 65-75 (32-5-35-5 per cent of the theoretical amount). 

The free base tends to become oxidized in the air but may be preserved as the hydrochloride. This is prepared by transferring it as soon as possible to 1500 cc. of distilled water containing 100 cc. of concentrated hydrochloric acid. The sparingly soluble hydrochloride separates at once. It is recrystallized from the mixture with the use of a little decolorizing carbon, whereupon it separates as colorless needles. A further crop is obtained on concentrating the mother liquor under reduced pressure to about 200 cc. The yield is no g. (82.1 per cent of the theoretical amount). 

The alcohol may be distilled from the mother liquor of the recrystallization. The residue from this distillation may be added to the mother liquor of the first crystallization, which is then concentrated to the crystallization point. The crop of crystals thus obtained will usually require double recrystallization. Alcohol recovered from the first mother liquor will contain too much volatile oil of nutmeg to be used for other purposes. 

On recovery of the tetrachloroethane by steam distillation of the mother liquor, there is obtained a small additional quantity of material (5 g.), but it is quite dark and of poor quality. 

The heptamethylene glycol was separated by continuous ether extraction from the alkaline reduction solution after the latter had been diluted and distilled to remove the alcohol. The nonamethylene glycol was separated from the alkaline liquor by decantation (as above) and distilled. All the others were crystallized from benzene (without alcohol). Equally successful results have also been obtained with larger runs (e.g., 0.5 mole of ester),... 

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