Year: 1899

page_text: We, CHARLES SUDRE, of 12, Boulevard St. Marcel, Engineer, and CHARLES
VICTOR THIERRY (signing as Ch. Thierry), of 11, Rue Meynadier, Engineer,
both in Paris, France, do hereby declare the nature of this invention to be
as follows:-
:―
It is known that the residues obtained from the distillation of wines, molasses,
grains, beet-roots, potatoes, and in general the residues from the distillation of
all materials which have undergone an alcoholic fermentation, contain glycerine,
nitric compounds, mineral substances, especially potash, and the like.
Numerous methods have already been proposed for treating these residues with
a view to obtaining as bye products of distillation, glycerine, nitric substances,
especially in the form of ammonia, tars and salts.
Among these methods the general process which however bas several modifi-
cations, consists in simply subjecting the residues to the action of heat under
conditions varying according to each modification.
Our improved process relates to this general process of treating by the action
of heat.
According to one method now known the concentrated residue is saturated
with lime, and the product is heated from the beginning of the operation, in
a vacuum preferably in the presence of superheated steam, this being done
particularly with a view to obtaining glycerine. But such process is impractic-
able, for the reason that in the vacuum under the action of heat, such a
quantity of gas or vapour is developed and such a turgidness and foaming
produced, that it is impossible and even dangerous to carry out this operation,
quite apart from its yielding no result whatever.
According to another known method the saturation is not effected by means
of lime, but, in order to avoid the foaming, the product is first heated up to
280 degrees Centigrade and the wash is then hastily boiled as it were. Iu
this process however the glycerine and a portion of the ammoniacal substances
and of the tars is lost.
The present process is based upon the observation that as glycerine kept
under atmospheric pressure can only be distilled at a temperature nearing 280
degrees, if the residues are first heated under atmospheric pressure up to about
200 degrees, wet steam ammoniacal substances, simple or compound and light
tars only are produced, but by this first operation exactly those substances are
expelled from the residue which caused the turgidness and foaming in the
vacuum,
The distillation of the glycerine in the vacuum may then be commenced without
Bu inconvenience

page_text: Thus the process consists in first concentrating the residues or mash up to
33 to 35 degrees Beaumé, and neutralising the same or not, for instance,
by means of lime. The distillation proper is then commenced and this up to
apont 110 degrees yields scarcely anything but water. The heat is then raised
to about 200 degrees care being taken to pass into the apparatus a current of
atmospheric air which carries away the substances decomposable between these
limits of temperature and which are more especially ammonia in simple or
compound form, which is collected in the sulphuric acid, and light tars.
In this operation the glycerine naturally is not distilled.
When those substances which are decomposable below 200 degrees Centigrade,
have been expelled, a vacuum is produced corresponding to about 20 millimetres
of mercury. The temperature is then preferably slightly reduced in order to be
subsequently again raised to about 200 degrees. During this period of dis-
tillation in the vacuum below 200 degrees, it is the glycerine that distils off;
and at the same time a little ammonia and tar is collected.
When the glycerine is nearly exhausted, the last traces are expelled by
sweeping the apparatus with a current of wet steam and the vacuum is destroyed.
The heat is then slowly and gradually continued until all ammoniacal sub-
stances and all heavy tars have been expelled, that is to say, until such heat
reaches about 500 to 600 degrees Centigrade.
All that is then left in the apparatus is carbonate and sulphate of potassium,
carbon and impurities.
The proportions of sulphate of potassium and of carbon are such that the
sulphate can be transformed into carbonate of potassium (which actually is of
a higher value) at a very low cost.
Dated this 14th day of November 1899.
PHILIP M. JUSTICE,
Chartered Patent Agent,
55 & 56, Chancery Lane, London,
For the Applicant.
An Improved Process for Treating Distillers Wash.
We, CHARLES SUDRE, of 12, Boulevard St. Marcel, Engineer, and CHARLES
VICTOR TILERRY (signing as Ch. Thierry), of 11, Rue Meynadier, Engineer,
both in Paris, France, do hereby declare the nature of this invention and in
what manner, the same is to be performed, to be particularly described and ascer-
tained in and by the following statement:-
It is known that the residues obtained from the distillation of wines, molasses,
grains, beet-roots, potatoes, and in general the residues from the distillation of
all materials which have undergone an alcoholic fermentation, contain glycerine,
nitric compounds, mineral substances, especially potash, and the like.
Numerous methods have already been proposed for treating these residues with
a view of obtaining as bye products of distillation, glycerine, nitric substances,
especially in the form of ammonia, tars and salts.
Among these methods the general process which however has several modifi-
cations, consists in simply subjecting the residues to the action of heat under
conditions varying according to each modification.

page_text: Our improved process relates to this general process of treating by the action
of heat.
According to one method now known the concentrated residue is saturated
with lime, and the product is heated from the beginning of the operation, in
a vacuum preferably in the presence of superheated steam, this being done
particularly with a view to obtaining glycerine. But such process is impractic-
able, for the reason that in the vacuum under the action of heat, such a
quantity of gas or vapour is developed and such a turgidness and foaming
produced, that it is impossible and even dangerous to carry out this operation,
quite apart from its yielding no result whatever.
According to another known method the saturation is not effected by means
of lime; but, in order to avoid the foaming, the process is first heated up to
280 degrees Centigrade and the wash is then hastily boiled as it were. In
this process however the glycerine and a portion of the ammoniacal substances
and of the tars is lost.
The present process is based upon the observation that as glycerine kept
under atmospheric pressure can only be distilled at a temperature nearing 280
degrees, if the residues are first heated under atmospheric pressure up to about
200 degrees, wet steam ammoniacal substances, simple or compound and light
tars only are produced, but by this first operation exactly those substances are
expelled from the residue which caused the turgidness and foaming in the
vacuum.
The distillation of the glycerine in the vacuum may then be commenced without
any inconvenience.
Thus the process consists in first concentrating the residues or wash up to
33 or 35 degrees Beaumé, and neutralising the same or not, for instance,
by means of lime. The distillation proper is then commenced and this up to
about 110 degrees yields scarcely anything but water. The heat is then raised
to about 200 degrees care being taken to pass into the apparatus a current of
atmospheric air which carries away the substances decomposable between these
limits of temperature and which are more especially ammonia in simple or
compound form, which is collected in the sulphuric acid, and light tars.
In this operation the glycerine naturally is not distilled.
When those substances which are decomposable below 200 degrees Centigrade,
have been expelled, a vacuum is produced corresponding to about 20 millimetres
of mercury. The temperature is then preferably slightly reduced in order to be
subsequently again raised to about 200 degrees. During this period of dis-
tillation in the vacuum below 200 degrees, it is the glycerine that distils off;
and at the same time a little ammonia and tar is collected.
When the glycerine is nearly exhausted, the last traces are expelled by
sweeping the apparatus with a current of wet steam and the vacuum is destroyed.
The heat is then slowly and gradually continued until all ammoniacal sub-
stances and all heavy tars have been expelled, that is to say, until such heat
reaches about 500 to 600 degrees Centigrade.
All that is then left in the apparatus is carbonate and sulphate of potassium,
carbon and impurities.
The proportions of sulphate of potassium and of carbon are such that the
sulphate can be transformed into carbonate of potassium (which actually is of
a higher value) at a very low cost.
Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed, I declare that what
I claim is: :-
The improved process for treating distillers wash consisting in first
concentrating the residues, and nentralizing them or not as desired,
then heating them in presence of a current of air to about 200° C.
for the purpose of evaporating the water and collecting some ammonia and light

page_text: tars, then heating them a second time to about 200° C. in a vacuum to collect
the glycerine some ammonia and the rest of the light tars then destroying the
vacuum and raising the heat to about 600° C. to collect the rest of the aminoniacal
substances and the heavy tars, substantially as described.
Dated this 25th day of July 1900.
PHILIP M. JUSTICE,
50 & 56, Chancery Lane, London,
Chartered Patent Agent,
For the Applicants.