Improved Process for the Manufacture of Alcohol by Saccharification and Fermentation by Mucedines, and Apparatus therefor.
Year: 1897

page_text: Date of Application, 28th Aug., 1897-Accepted, 12th Feb., 1898
Improved Process for the Manufacture of Alcohol by Saccharification
and Fermentation by Mucedines, and Apparatus therefor.
We, AUGUSTE COLLETTE FILS and AUGUSTE, BOIDIN, both of Seclin (Nord), in
the Republic of France, Distiller and Chemist respectively, do hereby declare the
nature of this invention and in what manner the same is to be performed, to be
particularly described and ascertained in and by the following statement:-
It is well known that in the manufacture of alcohol from grain only 75 to 80%
of the return which ought to be obtained, is actually obtained. Thus for 100
kilogrammes of starch capable of yielding theoretically 67:888 litres of alcohol
of 100 degrees, the treatment with acids only yields on an average 50 litres of
alcohol, and with malt only 55 litres, whilst the so-called Chinese process (see
Annals of the Pasteur Institute, Paris 1892, page 604) only yields 26 litres.
These poor results are justly attributed to the losses resulting from the intrusion
of micro-parasites which act during the fermentation and diminish, prevent, or
sometimes even destroy the products obtained by the industrial processes at present
employed. With the object of preventing this infection Dr. Effront has already
patented the use of hydrofluoric acid for rendering wort antiseptic, relying on the
fact that this acid is only slightly deleterious to alcoholic ferments whilst it has
an action on certain of the micro-parasites. In certain cases the said process appears
to have improved the returns to a considerable extent but not sufficiently for the
complete utilisation of the raw materials.
The ascertaining of this fact caused us to experiment in order to see if it were
not possible to approach more closely to a maximum return and this result we
have attained by utilising the saccharifying and fermenting properties of cer-
tain non-pathogenic mucedinere and more particularly those known as amylomiceæ
Rouxii (studied by Dr. Calmette, see Annals of the Institute Pasteur 1892 page 604
and 1897 page 264), the properties of the said mucedinere being utilised by effect-
ing the saccharification and fermentation in absolutely sterilised chambers and
under the special conditions hereinafter described.
It must first be stated that our improved process of utilising these mucedineæ
differs entirely from those proposed by Mr. Takamine for using the aspergillus
orize or koji. For instance Mr. Takamine in the Specification of his English
Patent No. 17277 % proposes the use of diastase precipitated by alcohol from cul-
tures of aspergillus on bran, the diastase thus purified being employed for the
direct saccharification of the grain.
Our process on the contrary is based on the direct saccharification and fermenta-
tion in sterilised chambers by the action of special mucedineæ alone or in
combination with certain kinds of yeast.
The various operations will now be described, the reasoning being pointed out
together with the facts ascertained from our industrial experiments and the uses
we make of them.
RENDERING THE WORT FLUID.

page_text: 4TH PROCESS.
The liquefaction of the starch may also be produced either by means of a vigor-
ous agitation or by the addition of a stirring apparatus to the fermenting vat.
The destruction of all the clots of starch which may become separated from the
liquid during the cooling is thus obtained.
It is important to note that in the four cases hereinbefore enumerated, it is
quite superfluous to produce the saccharification of the starch and that contrary
to what is done in the ordinary processes, it is sufficient to render the clots of
starch sufficiently fluid to prevent masses of amylum being deposited in the vat
where the saccharification herein before described is to be produced. It may also
be pointed out for that matter that the portion of saccharification which might
have been eventually produced during one of the said operations, could not in any
case be injurious to the final results.
SACCILARIFICATION AND FERMENTATION.
The fluid starch, diluted by the addition of warm water or low wines resulting
from a previous operation, is sterilised, that is to say it is brought to a pressure
of steam corresponding to the temperature at which the micro-organisms and their
germs are destroyed. This operation which takes place in the fermenting vat
also sterilises the interior of the latter and we take care to maintain the whole
protected from any contamination. This is obtained by preventing the re-entrance
into the vat of any solid or gaseous substance capable of conveying the micro-
organisms or germs capable of causing perturbations of any kind. In order to
obtain this we arrange our apparatus in such a way that there is constantly a pres-
sure of gas therein superior to the atmospheric pressure. We thus solve in a very

page_text: simple way one of the greatest difficulties of maintaining sterilising operations on
an industrial scale and we attach all the importance which it deserves to this
part of our process. The fluidified starch is then cooled to the temperature which
is best suited to the mucedineæ which it is desired to employ for the saccharifica-
tion.
The wort must also be brought to an acidity and concentration such that the
micro-organisms which may be employed may not be impeded nor paralysed either
by the acid remaining or by the alcohol produced during the fermentation. All the
conditions of acidity, temperature, concentration and sterilisation being fulfilled,
the wort is sprinkled (with all requisite precautions) with the saccharifying
mucedineæ, for instance with amylomiceæ Rouxii..
It is then strongly aerated with pure air to ensure the multiplication of the
plant. The air employed for this must be filtered and deprived of all matters
in suspension in an apparatus previously sterilised at a suitable temperature. A
mechanical agitator is employed for maintaining the sprinkled mucedineæ in the
mass of the liquid and for dividing it in order to ensure the greatest possible dis-
tribution of the mycelian tubes. Owing to the agitation and aeration under the
above named conditions, one gramme of mucedineæ operates on 300 hectolitres
of wort in 8 to 10 hours and produces the saccharification in less than 24 hours.
The sugar thus formed is soon converted into alcohol.
We have observed that this last transformation is accelerated if a very small
quantity of yeast is added to the vat.
In order to clearly establish the novelty of our inethod of operating, we will now'
give the following comparisons.
ADVANTAGES OF OUR PROCESS OVER THE ORDINARY METHOD OF WORKING
WITH MALT.
The process of manufacture is considerably simplified and is more easily carried
out because :
1st. The manufacture of yeast is suppressed and the loss resulting from the pro-
duction of lactic acid is therefore also dispensed with, as also that resulting from
the presence of non-saccharified starch in the said yeast.
2nd. The cost of preparing the malt and the loss of starch occasioned by the
germination and the micro-organisms which swarm on the surface of the malt are
almost entirely avoided.
3rd. The result is that the mucedine which we employ secrete saccharifying.
diastases, that the operation is carried on in the absence of any foreign ferment
and we thus suppress all acetic, lactic, butyric viscous or the like fermentations
which arise during the ordinary fermentations based on the use of malt. No pro-
cess hitherto exists which allows of a saccharification by means of diastases in a
sterilised chamber being obtained. It is owing to the purity of the fermentations
that we obtain alcohol of superior quality.
4th. The mucedineæ, which reproduce themselves to a large extent, fix on
themselves a portion of the soluble substances contained in the wort more par-
ticularly the nitrogen (certain mucedineæ contain 45% of their dry weight of
nitrogenous substances). We are thus able to increase the weight and quality of the
insoluble residues by the absorption of products held in solution.
5th. The mucedinem render the filtration very easy because they attack and
convert the gummy substances and because the mycelian tubes which they emit
and which branch (spread like hair) form a sort of felted matter assisting the
filtration. This filtration may be carried out either before or after the distillation.
We attach a considerable practical importance to this property peculiar to our
worts because one of the principal defects of working with malt is the production
of dregs difficult and frequently impossible to filter.
It is important also to point out that the use of mucedineæ is not dangerous
as they are not pathogenic, and they are also destroyed during the operations of
distillation.

page_text: ADVANTAGES OF OUR PROCESS OVER THE TREATMENT WITH ACIDS.
1st. The quantities of acid employed are insignificant affording a considerable
saving.
2nd. The formation of caramel in the juice and the losses of glucose due to the
virulent action of the acids employed in large doses is avoided.
3rd. The dissolution of the major part of the non-fermenting compounds is
avoided and the return of solid dregs is doubled and this whilst still preserving
their edible properties.
ADVANTAGES OF THE PROCESS OVER THE CHINESE PROCESS.
1st. The Chinese process cannot be employed when working on a large scale
and our method of working shows in comparison an enormous reduction in labour.
2nd. In order to allow of the growth being produced of the ferments which are
contained in the Chinese yeast, it is necessary to boil the rice very imperfectly
and the result is that when the fermentation is terminated there remains an in-
portant proportion of unattacked starch. This loss is entirely avoided by our
process.
وو
3rd. In the Chinese process a little known mixture of the various ferments which
the so-called "Chinese yeast contains is allowed to develop in the open air
resulting in an inevitable combustion of sugar formed, i.e., a conversion of the
saccharine substances into carbonic acid and water, without production of alcohol,
and under the influence of the air, which latter is indispensable for a combus-
tion."
«
In our process of working in hermetically closed vessels on the contrary, such
combustion is impossible and the admission of outer air may be dispensed with
as soon as the mucedineæ have obtained sufficient development.
4th. In following the prescriptions indicated by Dr. Calmette in his pamphlet
Manufacture of alcohol from rice in the Far East." (Fabrication des alcools de
ris en Extrême Orient), we have only obtained as a maximum 36 litres of alcohol
per 100 kilogrammes of rice, whilst by our process we obtain a minimum of 45
litres.
.
5th. The Chinese process yields dregs which cannot be filtered whilst our process
yields eminently filterable ones.
Finally our process gives greater returns than any other known processes and
yields alcohol of remarkable purity and also gives us an increased yield of richer
and more readily filtered dregs.
It will be understood that we may employ other saccharifying ferments such
as Aspergillus orizo (see Takamine's English patent aforesaid), chlamydomucor
orize (Went et Prinsen Geerbigs, see Archives of the Sugar Industry, Java, 1894),
the mucor alternans (Gayon see Annals of the Institute Pasteur 1887 page 532)
and the like, under similar conditions to those hereinbefore described for the
amylomnicea Rouxi, which has been selected by us because it has furnished the
best results.
In order to sum up we may state that our mode of working is based on the
saccharification and direct antiseptic fermentation by mucedineæ alone, or if neces-
sary in combination with slight quantities of yeast.
The mode of working comprises:
1. A liquefaction of the boiled amylaceous mass by a slight addition either of
acid, malt or culture of mucedinere, or of diastases of these mucedinese, or even
by a complete subdivision of the starch by agitation, trituration or mashing.
2. Boiling in order to ensure complete and perfect solubility or perfect and com-
plete dissolution of the amylums and in order to sterilise the wort in closed vessels
capable of being maintained sterilised such as described.
3. Cooling and aerating the wort with pure air and sprinkling or impregnating
it with the saccharifying mucedineæ in sterilised chambers.

page_text: 4. The saccharification and fermentation of the starch by the mucedineæ with the
optional addition of yeasts or suitable ferments.
5. Filtration of the dregs, which is rendered more easy owing to the properties
imparted to them by the mucedineæ.
Having now particularly described and ascertained the nature of our said Inven-
tion and in what manner the same is to be performed, we declare that what
we claim is:-
1. A process for the manufacture of alcohol characterised by the saccharifica-
tion being produced in sterilised chambers by means of the diastases of mucedineæ
such as the amylomicea Rouxii, aspergillus orizo, and by the saccharification and
fermentation being effected simultaneously, substantially as hereinbefore set forth.
2. A process for the manufacture of alcohol such as described characterised by
the suppression in said process of the combustions or conversions inevitable in
other processes based on the use of mucedineæ such as the Chinese process, the
maintenance of the mucedineæ in a submerged condition by agitation, and the
carrying out of the process in a closed vessel in which only as much air is admitted
as is necessary for the reproduction of the mucedinem utilised, whilst preventing
them producing aerial spores substantially as described.
Dated th
1907
WM. P. THOMPSON & Co.,
Of 6, Lord Street, Liverpool, Agents for the Applicants.