Title: A Practical Handbook on the Distillation of Alcohol from Farm Products
Author: F. B. Wright
Release date: July 23, 2014 [eBook #46377]
Most recently updated: October 24, 2024
Language: English
Credits: K. Nordquist, Sigal Alon, Jens Nordmann and the Online Distributed Proofreading Team
INCLUDING
The Processes of Malting; Mashing and Mascerating; Fermenting
and Distilling Alcohol from Grain, Beets,
Potatoes, Molasses, etc., with Chapters
on Alcoholometry and the
DE-NATURING OF ALCOHOL
FOR USE IN
Farm Engines, Automobiles, Launch Motors, and in Heating
and Lighting; with a Synopsis of the New Free
Alcohol Law and its Amendment and the
Government Regulations.
BY F. B. WRIGHT.
SECOND EDITION, REVISED AND GREATLY ENLARGED
NEW YORK
SPON & CHAMBERLAIN, 123 Liberty Street
LONDON
E. & F. N. SPON, Limited, 57 Haymarket, S.W.
1907
Copyright, 1906,
By SPON & CHAMBERLAIN.
Copyright, 1907,
By SPON & CHAMBERLAIN.
McIlroy & Emmet, Printers, 22 Thames St., New York, U. S. A.
Since the passage of the “Free Alcohol Act” there has been a constantly increasing demand for information as to the manufacture of industrial alcohol. This, with the favorable reception accorded to the first edition of this book has lead the publishers to bring out a second edition.
The entire volume has been carefully revised and not only has the original text been amplified but new chapters have been added explaining the most modern and approved methods and appliances both as used in Europe and in this country. Another valuable feature of the present volume is the collection of U. S. de-naturing formulas covering the special denaturants necessitated by the various arts and by the Government requirements. The chapters on modern distilling apparatus rectifiers and modern plants have been very carefully prepared in order to give the reader a clear idea of the various types of apparatus in use to-day and of their general place in a distillery system. The value of the book has been further increased by numerous additional illustrations.
It would be impossible in the compass of one small volume to describe all the practical details of alcohol manufacture particularly as these details vary with every distillery, but it has been the aim of the author to give sufficient information to enable every reader to understand the theory and general practice of the art, leading him from the simple methods and apparatus used until the last ten years to the more complicated stills and processes which have been lately devised.
Inasmuch as the manufacture of industrial alcohol has been most highly perfected in France and Germany, use has been made of the best European authorities and in particular the author begs to acknowledge his indebtedness to Sa Majeste L’Alcohol by L. Beaudry de Saunier. The publishers’ and author’s acknowledgements are also due to the Vulcan Copper Works Company of Cincinnati, Ohio, and to the Geo. L. Squier Manufacturing Company, Buffalo, New York, for their kindness in allowing illustrations to be given of modern American distilling apparatus.
F. B. Wright.
New York, Aug. 1, 1907.
To the majority of persons Alcohol connotes liquor. That it is used to some extent in the arts, that it is a fuel, is also common knowledge, but Alcohol as a source of power, as a substitute for gasoline, petroleum, and kindred hydrocarbons was hardly known to the generality of Americans until the passage of the “De-naturing Act” by the last Congress.
Then Alcohol leaped at once into fame,—not merely as the humble servant of the pocket lamp, nor as the Demon Rum, but as a substitute for all the various forms of cheap hydrocarbon fuels, and as a new farm product, a new means for turning the farmer’s grain, fruit, potatoes, etc., into that greatest of all Powers, Money.
That Alcohol was capable of this work was no new discovery accomplished by the fiat of Congress, but the Act of June 7, 1906, freed de-natured Alcohol from the disability it had previously labored under,—namely, the high internal revenue tax, and so cheapened its cost that it could be economically used for purposes in the arts and manufactures which the former tax forbade.
This Act then opens the door of a new market to the farmer and the manufacturer, and it is in answer to the increased desire for information as to the source of Alcohol and its preparation that this book has been written. The processes described are thoroughly reliable and are such as have the approval of experience.
As was stated above, Alcohol is not a natural product, but is formed by the decomposition of sugar or glucose through fermentation. This leaves Alcohol mixed with water, and these in turn are separated by distillation.
The literature treating of the distillation of Alcohol from farm products is very scant. But due credit is here given to the following foreign works which have been referred to: Spon’s Encyclopædia of the Industrial Arts, which also contains an article on Wood Alcohol, Mr. Bayley’s excellent Pocketbook for Chemists, and Mr. Noel Deerr’s fine work on Sugar and Sugar Cane.
New York
Oct. 31, 1906
| CHAPTER I. | |
| Alcohol, Its Various Forms and Sources. | |
| Its chemical structure. How produced. Boiling points. Alcohol and water. Alcohol, where found. Produced from decomposition of vegetables. Sources. Principal alcohols. | 1 |
| CHAPTER II. | |
| The Preparation of Mashes, and Fermentation. | |
| A synopsis of steps. Mashing starchy materials. Gelatinizing apparatus and processes. Saccharifying. Cooling the mash. Fermentation. Yeast and its preparation. Varieties of fermentation:—Alcoholic, acetous, lactic and viscous. Fermenting periods. Fermenting apparatus and rooms. Strengthening alcoholic liquors. | 8 |
| CHAPTER III. | |
| Distilling Apparatus. | |
| The simple still. Adams still. Concentrating stills. Compound distillation. Dorn’s still. Continuous distillation. The Cellier-Blumenthal still. Coffey’s still. Current stills. Regulating distillery fire. | 33 |
| CHAPTER IV.[viii] | |
| Modern Distilling Apparatus. | |
| The principles of modern compound stills. Vapor traps and their construction. Steam regulation. Feed regulation. American apparatus. The Guillaume inclined column still. | 66 |
| CHAPTER V. | |
| Rectification. | |
| General principles of “ractionation.” Old form of rectifying still. Simple fractionating apparatus. “Vulcan” rectifier. Barbet’s twin column rectifier. Guillaume’s “Agricultural” rectifying apparatus. Rectifying by filtration. | 82 |
| CHAPTER VI. | |
| Malting. | |
| The best barley to use. Washing. Steeping. Germinating. The “wet couch.” The “floors.” “Long malt.” Drying. Grinding and crushing. | 103 |
| CHAPTER VII. | |
| Alcohol from Potatoes. | |
| Washing. Gelatinizing and saccharifying. Low pressure steaming, and apparatus therefor. Crushing the potatoes. High pressure steaming and apparatus. The vacuum cooker. The Henze steamer. Isolation of starch without steam. English methods. Saccharifying the starch. | 110 |
| CHAPTER VIII.[ix] | |
| Alcohol from Grain, Corn, Wheat, Rice, and Other Cereals. | |
| Relative yields of various cereals. Choice of grain. Proportions of starch, etc., in various grains. Grinding. Steeping. Preparatory mashing. Saccharifying. Treatment of grain under high pressure. Softening grain by acid. | 126 |
| CHAPTER IX. | |
| Alcohol from Beets. | |
| Beet cultivation. Composition. Soil and manures. Sowing. Harvesting. Storing. Production of alcohol from beets. Cleaning and rasping. Extraction by pressure. Extraction by maceration and diffusion. The diffusion battery. Fermentation. Direct distillation of roots. | 140 |
| CHAPTER X. | |
| Alcohol from Molasses and Sugar Cane. | |
| The necessary qualities in molasses. Beet sugar. Molasses mixing and diluting. Neutralizing the wash. Pitching temperature. Distilling. Fermenting raw sugar. Cane sugar molasses. “Dunder.” Clarifying. Fermenting. Various processes. | 163 |
| CHAPTER XI. | |
| Alcoholometry. | |
| Hydrometers in general. Proof spirit. Syke’s hydrometer. Gay-Lussac’s hydrometer. Tralles alcoholometer. Hydrometric methods. Estimation of alcohol. Field’s alcoholometer. Grisler’s method and apparatus. Estimating sugar in mash. Determination of alcoholic fruits. Physical tests. Chemical tests. The Permanganate of Potash test. Results by Barbet. | 174 |
| CHAPTER XII. | |
| Distilling Plants, Their General Arrangement and Equipment. | |
| Simple apparatus. Elaborate plants. Steam stills. The fermenting room. Ventilation. Fermenting vats. Preparatory vats. Arrangement of grain distillery. A small beet distillery. Large beet distilling plant. Transporting beets. Potato distillery. Molasses distillery. Fermenting house for molasses. Transportation of molasses to distillery. Coal consumption. | 189 |
| CHAPTER XIII. | |
| De-natured Alcohol, and De-naturing Formulæ. | |
| Uses of alcohol. De-natured spirit:—Its use in Germany, France and England. The “Denaturing Act.” The uses of de-natured alcohol. Methods and Formulæ for de-naturing. De-natured alcohol in the industrial world. | 211 |
| CHAPTER XIV. | |
| De-naturing Regulations in the United States. | |
| The Free Alcohol Act of 1906, and proposed changes therein. The Amendment of 1907. Internal Revenue Regulations. | 224 |
| Index. | 261 |
| No. | Page. | |
| 1 | Vacuum mash cooker | 10 |
| 2 | Henze steamer | 12 |
| 3 | Mash cooler, air system | 15 |
| 4 | Mash cooler, water system | 17 |
| 5 | Yeasting and fermenting apparatus | 22 |
| 6 | A simple still | 34 |
| 7 | Simple direct-heated still | 35 |
| 8 | Simple still, with rectifier | 37 |
| 9 | Adam’s still | 39 |
| 10 | Corty’s simplified distilling apparatus | 41 |
| 11 | Double still | 42 |
| 12 | Dorn’s compound still | 43 |
| 13 | Compound still | 46 |
| 14 | Compound direct-fire still | 47 |
| 15 | Cellier-Blumenthal still | 49 |
| 16 | Details of rectifier column | 50 |
| 17 | Details of condenser and mash heater | 52 |
| 18 | Coffey’s rectifying still | 55 |
| 19, 20 | Rotary current still | 59, 60 |
| 21 | Indicator for regulating the distilling fire | 61 |
| 22 | Diagrammatic view of column still and accessory apparatus | to face 64 |
| 23 | Distilling plate | 64 |
| 24, 25 | Barbet traps | 68 |
| 26 | Steam regulator | 70 |
| 27 | Gauge glass for regulator | 72 |
| 28 | Continuous distilling apparatus with external tubular condenser | 72 |
| 29 | Detail of chamber, continuous still | 73 |
| 30, 31 | Details of perforated plate A | 75, 76 |
| 32 | Continuous distilling apparatus with goose separator | 76 |
| 33 | Section of Gillaume’s inclined column still | 78 |
| 34 | Gillaume’s inclined column still | 79 |
| 35 | Rectifying still | 88 |
| 36 | Section of rectifying still | 89 |
| 37 | Fractional distilling apparatus | 91 |
| 38 | Rectifying apparatus with external tubular condenser | 94 |
| 39 | Twin column Barbet rectifier | 95 |
| 40 | Gillaume’s rectifier and inclined still | 97 |
| 41 | Steaming vat for potatoes | 112 |
| 42 | Bottom of steaming vat | 113 |
| 43 | Steam generator | 114 |
| 44 | Potato steamer and crusher | 116 |
| 45 | Bohn’s steamer and crusher | 118 |
| 46 | Stack for storing beets | 148 |
| 47 | Storage cellar for beets | 149 |
| 48 | Beet and potato rasp | 152 |
| 49 | Dujardin’s roll press | 155 |
| 50 | Defusion battery | 158 |
| 51 | Mixing vat | 165 |
| 52 | Syke’s hydrometer | 176 |
| 53 | Field’s alcoholometer | 182 |
| 54 | Geisler’s apparatus | 184 |
| 55 | Continuous grain alcohol distillery—Barbet’s system | 198 |
| 56 | Grain distillery, capacity 2500 bushels per day | 198 |
| 57 | Small beet distillery | 200 |
| 58 | Large beet distillery | 202 |
| 59 | Molasses distillery, capacity 2500 gallons per day | 206 |
| 60 | Molasses fermenting house | 207 |
Alcohol. (Fr., alcool; Ger., alkohol.) Formula, C2H6O.
Pure alcohol is a liquid substance, composed of carbon, hydrogen, and oxygen, in the following proportions:
| C | 52.17 |
| H | 13.04 |
| O | 34.79 |
| 100.00 |
It is the most important member of an important series of organic compounds, all of which resemble each other closely, and possess many analogous properties. They are classed by the chemist under the generic title of “Alcohols.”
Alcohol does not occur in nature; it is the product of the decomposition of sugar, or, more properly, of glucose, which, under the influence of certain organic, nitrogenous substances, called ferments is split up into alcohol and carbonic anhydride. The latter is evolved in the form of gas, alcohol remaining behind mixed with water, from which it is separated by distillation. The necessary purification is effected in a variety of ways.
Table I.—The Boiling Points of Alcoholic Liquors of Different Strengths, and the Proportions of Alcohol in the Vapors Given Off.
| Proportion of alcohol in the boiling liquid in 100 vols. |
Temperature of the boiling liquid. |
Proportion of alcohol in the condensed vapor in 100 vols. |
Proportion of alcohol in the boiling liquid in 100 vols. |
Temperature of the boiling liquid. |
Proportion of alcohol in the condensed vapor in 100 vols. |
| 92 | 171.0 F. | 93 | 20 | 189.5 F. | 71 |
| 90 | 171.5 F. | 92 | 18 | 191.6 F. | 68 |
| 85 | 172.0 F. | 91.5 | 15 | 194.0 F. | 66 |
| 80 | 172.7 F. | 90.5 | 12 | 196.1 F. | 61 |
| 75 | 173.6 F. | 90 | 10 | 198.5 F. | 55 |
| 70 | 175.0 F. | 89 | 7 | 200.6 F. | 50 |
| 65 | 176.0 F. | 87 | 5 | 203.0 F. | 42 |
| 50 | 178.1 F. | 85 | 3 | 205.1 F. | 36 |
| 40 | 180.5 F. | 82 | 2 | 207.5 F. | 28 |
| 35 | 182.6 F. | 80 | 1 | 209.9 F. | 13 |
| 30 | 185.0 F. | 78 | 0 | 212.0 F. | 0 |
| 25 | 187.1 F. | 76 |
Pure, absolute alcohol is a colorless, mobile, very volatile liquid, having a hot, burning taste, and a pungent and somewhat agreeable odor. It is very inflammable, burning in the air with a bluish-yellow flame, evolving much heat, leaving no residue, and forming vapors of carbonic anhydride and water. Its specific gravity at 0° C (32° F.) is .8095, and at 15.5° C. (60° F.) .794; that of its vapor is 1.613. It boils at 78.4° C. (173° F.). The boiling point of its aqueous mixtures are raised in proportion to the quantity of water present. Mixtures of alcohol and water when boiled give off at first a vapor rich in alcohol, and containing but little aqueous vapor; if the ebullition be continued a point is ultimately reached when all the alcohol has been driven off and nothing but pure water remains. Thus, by repeated distillations alcohol may be obtained from its mixtures with water in an almost anhydrous state.
Absolute alcohol has a strong affinity for water. It absorbes moisture from the air rapidly, and thereby becomes gradually weaker; it should therefore be kept in tightly-stoppered bottles. When brought into contact with animal tissues, it deprives them of the water necessary for their constitution, and acts in this way as an energetic poison. Considerable heat is disengaged when alcohol and water are brought together; if, however, ice be substituted for water, heat is absorbed, owing to the immediate and rapid conversion of the ice into the liquid state. When one part of snow is mixed with two parts of alcohol, a temperature as low as 5.8° F. below zero is reached.
When alcohol and water are mixed together the resulting liquid occupies, after agitation, a less volume than the sum of the two original liquids. This contraction is greatest when the mixture is made in the proportion of 52.3 volumes of alcohol and 47.7 volumes of water, the result being, instead of 100 volumes, 96.35. A careful examination of the liquid when it is being agitated reveals a vast number of minute air-bubbles, which are discharged from every point of the mixture. This is due to the fact that gases which are held in solution by the alcohol and water separately are less soluble when the two are brought together; and the contraction described above is the natural result of the disengagement of such dissolved gases. The following table represents the contraction undergone by different mixtures of absolute alcohol and water.
Table II.—100 Volumes of Mixture at 59° F.
| Alcohol. | Contraction | Alcohol. | Contraction | Alcohol. | Contraction |
| 100 | 0.00 | 65 | 3.61 | 30 | 2.72 |
| 95 | 1.18 | 60 | 3.73 | 25 | 2.24 |
| 90 | 1.94 | 55 | 3.77 | 20 | 1.72 |
| 85 | 2.47 | 50 | 3.74 | 15 | 1.20 |
| 80 | 2.87 | 45 | 3.64 | 10 | 0.72 |
| 75 | 3.19 | 40 | 3.44 | 5 | 0.31 |
| 70 | 3.44 | 35 | 3.14 |
Alcohol is termed “absolute” when it has been deprived of every trace of water, and when its composition is exactly expressed by its chemical formula. To obtain it in this state it must be subjected to a series of delicate operations in the laboratory, which it would be impossible to perform on an industrial scale. In commerce it is known only in a state of greater or less dilution.
Alcohol possesses the power of dissolving a large number of substances insoluble in water and acids, such as many inorganic salts, phosphorus, sulphur, iodine, resins, essential oils, fats, coloring matters, etc. It precipitates albumen, gelatine, starch, gum, and other substances from their solutions. These properties render it an invaluable agent in the hands of the chemist.
Alcohol is found in, and may be obtained from, all substances—vegetable or other—which contain sugar. As stated above, it does not exist in these in the natural state, but is the product of the decomposition by fermentation of the saccharine principle contained therein; this decomposition yields the spirit in a very dilute state, but it is readily separated from the water with which it is mixed by processes of distillation, which will subsequently be described. The amount of alcohol which may be obtained from the different unfermented substances which yield it varies considerably, depending entirely upon the quantity of sugar which they contain.
Alcohol is produced either from raw materials containing starch, as potatoes, corn, barley, etc., or raw materials containing sugar, as grapes, beets, sugar-cane, etc.
The following are some of the most important sources from which alcohol is obtained: Grapes, apricots, cherries, peaches, currents, gooseberries, raspberries, strawberries, figs, plums, bananas, and many tropical fruits, artichokes, potatoes, carrots, turnips, beet-root, sweet corn, rice and other grains. Sugar-cane refuse, sorgum, molasses, wood, paper, and by a new French process from acetylene. On a large scale alcohol is usually obtained from sugar beets, molasses or the starch contained in potatoes, corn and other grains. The starch is converted into maltose by mixing with an infusion of malt. The maltose is then fermented by yeast. Sulphuric acid may be used to convert even woody fibre, paper, linen, etc., into glucose, which may in turn be converted into alcohol.
Table III.—Principal Alcohols.
| Chemical Name. | Source. | Formula. | Boiling Point °F. | ||||
| 1 | Methyl | Alcohol | Distillation of Wood | CH3OH | 150.8 | ||
| 2 | Ethyl | “ | Fermentation | of | sugar | C2H5OH | 172.4 |
| 3 | Propyl | “ | “ | “ | grapes | C3H7OH | 206.6 |
| 4 | Butyl | “ | “ | “ | beets | C4H9OH | 242.6 |
| 5 | Amyl | “ | “ | “ | potatoes | C5H11OH | 278.6 |
| 6 | Caproyl | “ | “ | “ | grapes | C6H13OH | 314.6 |
| 7 | Aenanthyl | “ | Distillation castor oil with potatoes |
C7H15OH | 347.0 | ||
| 8 | Capryl | “ | Essential oil hog weed | C8H17OH | 375.8 | ||
| 9 | Nonyl | “ | Nonane from petroleum | C9H19OH | |||
| 10 | Rutyl | “ | Oil of Rue | C10H21OH | |||
| 11 | Cytyl | “ | Spermaceti | C16H33OH | |||
| 12 | Ceryl | “ | Chinese wax | C26H53OH | |||
| 13 | Melisyl | “ | Bees’ wax | C30H61OH | |||
Among a variety of other substances which have been and are still used for the production of alcohol in smaller quantities, are roots of many kinds, such as those of asphodel, madder, etc. Seeds and nuts have been made to yield it. It will thus be seen that the sources of this substance are practically innumerable; anything, in fact, which contains or can be converted into sugar is what is termed “alcoholisable.”
Alcohol has become a substance of such prime necessity in the arts and manufactures, and in one form or another enter so largely into the composition of the common beverages consumed by all classes of people that its manufacture must, of necessity, rank among the most important industries of this and other lands.
Of the alcohols given in the above table only two concern the ordinary distiller, or producer of alcohol for general use in the arts. Methyl alcohol, the ordinary “wood alcohol,” or wood naphtha, and Ethyl alcohol, which is produced by the fermentation of sugar and may therefore be made from anything which contains sugar.
Ethyl alcohol forms the subject of this treatise. Aside from its chemical use in the arts as a source of energy and as a fuel, alcohol will likely soon compete with petroleum, gasoline, kerosene, etc., under the Act of Congress freeing the “de-naturized” spirit from the Internal Revenue tax. This act and the de-naturing process are covered in the last chapters of this book.
Alcohol may be produced either from, (1) farinacious materials, such as potatoes or grains, (2), from sacchariferous substances such as grapes, sugar beets, sugar cane, or the molasses produced in sugar manufacture.
THE PREPARATION OF STARCHY MATERIALS.
Saccharification. Preparatory Mashing. With starchy materials it is first necessary to convert the starch into a sugar from which alcohol can be produced by the process of fermentation. This is called saccharification.
Gelatinizing. The first step in this process is gelatinizing the starch;—that is, forming it into a paste by heating it with water, or into a liquid mass by steaming it under high pressure. The liquid or semi-liquid mass is then run into a preparatory mash vat and cooled.
Saccharifying. The disintegrated raw materials or gelatinized starch in the preparatory mash vat is now to be “saccharified” or converted into sugar. This is effected by allowing malt to act on the starch. This malt contains a certain chemical “ferment” or enzyme, called “diastase” (“I separate”).
This is able under proper conditions to break up the gelatinized starch into simpler substances—the dextrins—and later into a fermentable sugar called maltose.
Fermentation.—The maltose or sugar in the “mash” is now to be converted into alcohol. This is accomplished by fermentation, a process of decomposition which converts the sugar into carbonic acid and alcohol. Fermentation is started by yeast, a fungus growth, which in the course of its life history produces a matter called zymose which chemically acts on the sugar to split it up into carbonic acid gas and alcohol.
Yeast may be either “wild” or cultivated. If the mash is left to stand under proper condition the wild yeast spores in the air, will soon settle in the mash and begin to multiply. This method of fermentation is bad because other organisms than yeast will also be developed,—organisms antagonistic to proper fermentation. As a consequence, pure or cultivated yeast is alone used.
This yeast is cultivated from a mother bed in a special yeast mash and when ripened is mixed with the mash in the fermenting vat. At a temperature between 50° F. and 86° F. the yeast induces fermentation, converting the sugar of the mash into carbon dioxid which escapes, and alcohol which remains in the decomposed mash, or “beer” as it is termed in the United States.
It now remains to separate the alcohol from the water of the beer with which it is mixed. This is accomplished by distillation and rectification, as will be fully described in the chapters following.
PRODUCTION OF ALCOHOL FROM SACCHARIFEROUS SUBSTANCES.
Substances such as grape juice, fruit juice, sugar beets, cane sugar and molasses already contain fermentable sugar. Saccharification is therefore not needed and juices or liquids from these matters are either directly fermented as in the case of sugar cane, or—as in the case of sugar beets—the sugar in juice is transferred by yeast into a fermentable sugar.
MASHING STARCHY MATERIALS.
We will now consider in more detail the preparation of mashes from starch-containing substances.
Gelatinizing Apparatus. These comprise either ordinary vats, into which steam at low pressure is admitted (see Fig. 44), cookers and stirrers such as shown in Fig. 1 and 45 or the Henze steamer (Fig. 2.)