UNITED STATES‘ PATENT ornron HABRYo. GHUTE, or CLEVELAND, oHIo. PROCESS OF PREPARING WOOD-ALCOHOL AND’ GH'LOROFORMLv

No. 893,784. Speci?cation of Letters Patent. Patented July 21, 1908. Application ?led October 6,‘ 1903. Serial No. 175,726.

' To all whom it may concern: physical aflinity for methyl alcohol and raise Be it known that I, HARRY 0. Errors, a its boiling point material , while having no citizen of the United States, and a resident such effect u on chloroform, chloroform be 55 of Cleveland, in the county of Cuyahoga and ing immiscilile with water and dissolving State of Ohio, have invented a new and Im few or none of the ordinary metallic salts. proved Process of Preparing woodeAlcohol Such an addition of water or soluble salts to and Chloroform, of which the following is a the reaction mixture tends to make the chlo full, clear, and exact description. roform se arate physicall from the methyl (30 This invention relates to processes of pre alcohol. ile nearly a soluble salts have 10 paring wood alcohol and chloroform; and this effect, the ordinary hygrosco ic salts com rises a method wherein pure wood or have it in an enhanced degree, nearlly all hy met yl alcohol and chloroform are separated grosco ic salts being quite soluble in methyl from each other by fractional distillation alcoho and its aqueous solutions. Using from a'mixture of the same after addition to water alone, I ?nd a useful degree of dilution 15 such mixture of one or more bodies having to be thatwhich will give an apparent alco the property of raising the boiling point of holic strength to the reaction mixture of such methyl alcohol and wherein such a mix about 50 er cent, although of course a ture is produced by treating ordinary crude greater or ess degree may be em loyed. A wood spirit with rea ents adapted to form dilution at which the mixture will) have such 20 chloroform therein; a l as more fully herein a specific gravity that upon spindlinc' with an after set forth and as claimed. or inary alcohol hydrometer it will show a Ordinary crude wood spirit, or the spirit-' reading of-about 50 per cent. alcohol is well uous roduct from the destructive distilla ada ted however to the present purposes. tion of wood and woody ?ber, consists essen A most any of the ordinary soluble or 25 tially of a mixture of methyl alcohol, acetone hygroscopic salts may be employed; such as, and other ketones, and other impurities, all for instance, potassium chlorid, potassium admixed with more or less water. Prepara nitrate, potassium acetate, sodium chlorid, tion of pure methyl alcohol from this crude sodium nitrate, sodium acetate and similar 80 wood spirit by the ordinary methods of frac salts of magnesium, calcium, barium, stron~ 30 tional distillation is a di?icult, tedious and tium and zinc. Of these salts, I prefer cal— expensive operation, the boiling‘ oints of cium chlorid as bein cheap, effective and the alcohol and of acetone lying not ar apart, easily regenerated. , n employing ordinary with those of other ketones and impurities bleaching powder, or calcium hypochlorite, 85 intermediate. . For this reason pure acetone to form a mixture of methyl alcohol and free methyl alcohol is unduly expensive in chloroform from crude wood spirit more or

commerce. ' . less calcium chlorid is formed in the reaction By treatment of wood alcohol with neu mixture. Where both water and salts are tral or alkaline hypochlorites, the acetone employed to raise the boiling point of methyl 90 and some of the other impurities are chan ed alcohol, the amount of water may be dimin 40 into chloroform, leaving the methyl alco o1 ished to correspond with the amount of salts unaltered, ‘provided there is no excess of hy present; 5'to 10 per cent. of calcium chlorid, ochlorite added. This is not in itself a use for instance,_-being used with a solution hav ul reaction, so far as previous knowledge has ing an apparent alcoholic tenor of 60 per 95 gone, for it is‘ di?icult to separate these cent. > ' 45 bodies by fractional distillation, the boiling ' In treating w'ood spirit with hypochlorites, oint of methyl alcohol, 66° 0., not being far ordinarily I prefer to use the calcium salt, or vfrom that of chloroform, 61° C. ordinary bleaching powder, as the cheapest, I have discovered that the addition of but other hypochlorites such as those of so 100 water or of soluble or hygroscopic salts, or of dium or potassium, may be employed. It is 50 both, converts this reaction mixture into one not necessary that the hypochlorite be pre from which the constituents can be easily formed since it can be generated in the reac separated. Water and such, salts possess a tion liquor itself, as by introducing chlorin 893,784

after making such liquor alkaline. It is im water yields its chloroform to distillation ?rst portant that the hypochlorite shall be pres and any such mixture may of course be treat 65 ent in‘a neutral or alkaline liquor, as hy o ed by'the described rocess. chlorites cannot exist in the resence of ree As‘ an example‘ 0 my process in treating acid but evolve'chlorin. . C lorin does not wood spirit,‘ I may run, say, 300 gallons of form chloroform but produces chlor-ace ‘wood spirit into a still of 1,000 gallons ca tones, bodies of higher boiling point and pacity. The s irit should preferably show 70 piercing odor. The reaction mixture con an apparent acoholic readin of about 95 taining the hypochlorite should be heated. er cent. on a Tralles alcoho ometer. The 10 Since wood spirit contains other bodies ralles scale is designed for grain alcohol but than acetone capable of reacting with hypo the speci?c gravities of methyl alcohol and chlorites, it is generally desirable only to add acetone solutions are about the same as those 75 the amount of such hypochlorite ca able of of grain alcohol. The spiritin the still is then reacting with such acetone, there y ‘both heated and a solution or pasty mixture con economizino' hypochlorite and securing purer taining the amount of hypochlorite deter ' roducts. zllor this urpose advantage may mined in the described manner as re uired e taken of the Wea (er a?inity of iodin for for that particular spirit, is next adde . As these other bodies. A measured portion of the reaction of the hypochlorite upon the the Wood spirit to be treated ma have added wood spirit evolves heat, care should be 20 to it an amount of potassium io id more than taken to prevent too ‘violent an action, as in is equivalent to the amount of acetone this event some of the methyl alcohol might likely to be present. Upon now- gradually ,be destroyed. When the action slackens, 85 adding a hy ochlorite solution of known 'water is added in amount su?icient' to give strength, the iodin and acetone react to form the liquid an apparent alcoholic strength of - iodoform and at the moment when the ace about 50 per cent. and heat is applied to dis tone all disappears, free iodin will be liber til off the chloroform which has been pro ated and may be detected. The amount of duced. As long as the distillate upon the 90 hy ochlorite necessary to produce this result addition of'water shows the presence of chlo is tllie most advantageous amount with which roform b forming a heavy underlying layer, 30 to treat the particular wood spirit under ex the disti late is caught in as ecial chloro amination. Or, 'after adding the potassium form receiver. When chloro orm will no iodid an excess of hypochlorite may be added lon er se arate, the distillation is continued 95 and the freed iodin titrated back in the ordi an ‘the istillate received in a tank for puri nary manner, the amount of such iodin corre ?ed methyl alcohol. 35 sponding to the excess of h‘ ochlorite which Having thus described my invention,v was employed. Upon ad 'ng the deter what I claim is :— mined amount of hypochlorite to a particu 1. The process of purifying Wood spirit 100 lar sample of wood s irit, the‘ acetone and which consists in treatlng wood spirit Wltll‘?. other chlorofornryiel ing ketones and‘ bod hypochlorite to; form ‘chloroform ‘from the 40 ies are converted while the remainin

which consists in diluting admixture of methyl In testimony whereof I have signed my . alcohol and chloroformwith water and dis- name to this speci?cation in the presence of 10 tilling off the chloroform. 1 two Witnesses. 6. In the process of purifying methyl a — ' cohol and ~producin chloroform, the method H‘ 0' OHUTE' which consists in di uting amixture of methyl Witnesses: alcohol and chloroform with water contain- H. L. PAYNE, ing a salt and distilling off the chloroform. W. P. JOHNSON.