Improvements in the Manufacture of Aethyl-alcohol.
Year: 1897

page_text: Date of Application, 24th Sept., 1897-Accepted, 20th Nov.,
1897
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Aethyl-alcohol.
I, EMIL ZDAREK of No. 13 Alserstrasse, Wien IX Austria, Chemist, do hereby
declare the nature of this invention and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement:-
This invention relates to a method of manufacturing acthyl-alcohol from cellu-
lose or wood and consists chiefly in the manner in which the inversion is performed,
in removing the vinegar-and levulinic acids as well as the empyreumatic (burned)
substances resulting from the inversion before fermentation of the inverted wood
substances & thus ferment and distil the inverted substance after the said
separation.
In carrying out this invention a quantity of acid equal to 1/10—3 per cent. of
the weight per cent. of the mash water is mixed with the mashed wood substance.
Any kind of acid may be used for the said purpose, preferably. sulphuric acid
and sulphuricacidanhydride which may be used separately or jointly.
When using sulphuricacidanhydride it is advisable to add nitric acid in quantity
of 1/100-5 per cent. of the weight of the sulphuricacid anhydride.
For the purpose of inversion into a substance capable of fermentation the
acidilated mash substance is then boiled in a closed vessel at a temperature of
130-170 degrees centigrade for a time varying between 1/4-3 hours according
to the nature of the wood and such a quantity of inactive gas injected during the
process of boiling, that the pressure existing in the said vessel exceeds that which
is equal to the temperature of the contents of the vessel one half-two atmospheres.
In further treating the inverted substance the chief object is to remove thu
bodies unfavourable for the process of fermentation and resulting from the process
of inversion, such as vinegar acid levulinic acid and empyreumatic substances,
which according to this invention may be effected by various methods such as
hereinafter successively described.
I METHOD.
After having completed the inversion, the sulphuric acid contained in the mash
substance is ascertained and a quantity of lime added necessary for the complete
neutralization of the sulphuric acid.
The mash free of sulphuric acid is heated in a closed vessel above the evapora-
tion point of the vinegar acid and the main part of the pyreumatic substances,
say to about 118-130 degrees, and the vapours resulting therefrom are allowed
to escape through an opening controlled by a tap or to pass into a vessel.
If levulinic acid is forming during the inversion, as is the case by certain kinds
of wood it is split before the said second boiling into vinegar acid and smaller
quantities of other organic acids, such as amber-and oxalic acid, by the calculated
quantity of nitric acid and the vinegar acid resulting therefrom simultaneously
removed with the vinegar acid formed in the product at the beginning, in the

page_text: II METHOD.
Instead of separating the vinegar acid, levulinic acid and empyreumatic sub-
stances from the mash by a second-boiling and the ejection of the vapours, these
acids may be split by neutralization with an excess of lime, whereby acetate-
and levulinate--of calcium besides sulfate of calcium is obtained; after neutraliza-
tion the products formed and the empyreumatic substances are electrolytically
split, that is to say, into carbonic acid, acthane and lime, which latter, after having
been converted into calciumhydroxyd and then into carbonate of lime, together
with the previously formed gypsum, constitutes a slimy sediment not soluble
whilst aethane and carbonic acid escapes from the mash. The apparatus used
and method in which the said electrolysis is performed is identical with that
generally used for treating liquids electrolytically.
The mash freed from the mineral and organic acids and burned substances in
one of the said manners, may be again neutralized and concentrated, by adding
alkali, amonia or lime, the residual empyreumatic substances if present escaping,
and after having been mixed with yeast is fermented and the aethyl-alcohol
obtained therefrom in the usual manner by distillation.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed, I declare that what I
claim is:
1 A method of manufacturing acthyl-alcohol from cellulose or wood, consisting
chiefly in boiling the wood mashed in water with sulphuric acid or sulphuricacidan-
hydride in quantity equal to 1/10-3 per cent. of the weight of the mash or with
a mixture of both these acids, from 1/4-3 hours at a temperature of about 130-
170 degrees, the pressure in the respective boiler being kept about at 1/2-2 atmo-
spheres above that which corresponds with the temperature in the boiler, by forcing
in or injecting an inactive gas and after having effected the inversion by boiling,.
removing the acids contained in the mash and empyreumatic substances either:-
a by introducing into the mash substance a quantity of lime which neutralizes
only the free sulphuric acid present and afterwards boiling it at a tempera-
ture of 118 130 degrees for the purpose of removing the vinegar acid and
empyreumatic substances, at the same time permitting the vapours to escape,
whilst before boiling the levulinic acid, which may exist in the mash, is
split by the addition of HNO 3 into vinegar acid and other organic acids or
bby neutralizing or converting the the organic and inorganic acids contained
in the mash into their lime salts by an excess of lime and separating by
electrolysis the acetate-and levulinate-lime thus obtained together with
the empyreumatic substances into carbonic acid and aethane, which escape
at once, and pure lime which after conversion into calciumhydrooxyd or
calciumcarbonate by the gypsum formed by the neutralization of the
sulphuric acid, forms a slimy sediment not soluble and finally obtaining
the eathyl-alcohol from the mash prepared in the manner as specified in
sub claim a or 6 by concentrating, fermenting and distilling the same, all.
substantially as set forth.
2). In the method described in Claim 1, the union with sulphuricacidanhydride
if used, of 0, 01-5 per cent. of the weight thereof of nitric acid during the first
inversion boiling, all substantially as set forth.
Dated this 22nd day of September 1897
F. BOSSHARDT & Co.,
Agents for Applicant.