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Jan. 7, 1947.
2,413,699
A. L. SCHADEv
PROCESS FOR THE FERMENTATION OF IMPURE} SUGAR SOLUTIONS
' Filed July 17, 1945
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INVENTOR
JVRn/z/R L. Sell/LUZ
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BY
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ATTORNEYS
2,413,699
Patented Jan. 7, 1947v
UNITED] STATES PATENT orrlcs
PROCESS FOR THE FERMENTATION 0F
IMPURE SUGAR SOLUTIONS
Arthur
Schade, New York, N. Y., assig'nor-to
The Overly Bio-‘Chemical Research Founda
tion, Inc., New York, N. Y., a corporation 0
New York
Application July '1, 1943, Serial No. 49544.6
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l
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8Claims.
(Cl.195—38)'
2
a
My invention relates to' the manufacture of
the fermentation, converted into insoluble mate
glycerine by the alkaline fermentation of sac
rials, so that they can be readily filtered off or _
- otherwise physically separated with the yeast.
It is a stillfurther object of the invention to
provide a steered fermentation'process wherein
chari?ed starchy materials.
It is the general object of the invention to pro;
vide an improved method for effecting the fer
mentation of hydrolyzed starchy materials
whereby a puri?ed fermentation liquor is obtained
‘the steering agent is of limited solubility and
forms an insoluble reaction product with carbon
dioxide so that it precipitates out of solution‘
during the course of the fermentation. Other
Attempts to produce glycerine by modi?ed 10 objects of the invention will become apparent as
from which the glycerine content can be more
' easily separated than heretofore.
alcoholic fermentation of sacchari?ed starchy
materials have not been commercially success
the, more detailed description of the invention
ful up to the present time. The major di?lculty
I have found that the various and diverse ob
jects of the invention can be attained by the use
proceeds.
'
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.
of the known processes has consisted in the re.
covery of the glycerine after the fermentation. 15 of calcium hydroxide as the alkalinizing or steer
This recovery has been serioushr hampered by 7, ing agent in the fermentation by yeast of sac
chari?ed starchy ‘materials and in general of
the fact that the known fermentation liquors
contain large amounts of impurities which could’
fermentable solutions containing also non-fer-v
not be removedeconomically and which gave
mentable polysaccharides, and proteins and pro
rise to considerable loss of glycerine on heating 20 tein-like substances. Calcium hydroxide appears
to presentan. almost ideal alkalinizing agent for
the concentrated slops. .
Among the impurities contained in the fer
complex. mixtures of this type because in addi
tion to being capable of maintaining the pH value
mentation liquors resulting from the known
processes are unfermentable polysaccharides. and
within the preferredwrange of about 7.5 to about
also various proteins or protein-like substances. 25 8.9, it is able, on the one hand,,to form com
. These materials remain in solution after the ?l
pounds with polysaccharides and proteins and
tration of the yeast, and as the glycerine is
protein-like substances which are insoluble under
alkaline conditions, and on the other hand to
usually recovered by distillation, these impurities
become more and more concentrated in the solu
tion in the still, and ultimately become very di?lcult to handle, and as a considerable portion
"of the glycerine remains in the still residue, the
form the insoluble calcium carbonate with car- _
bon dioxide. Consequently, the calcium hydrox
ide not only removes organic impurities from the
fermentation liquor but at the same time prevents
loss of glycerine in such residue becomes an im
an accumulation of soluble salts therein.
portant factor in the economy of the process.
A further difficulty arises by reason of the fact
improved process, therefore, the glycerine is pro
duced from sacchari?ed starchy materials and
equivalent; mixtures in high yields, and at the same
time the fermentation results in an at least par
tially puri?ed liquor from which the glycerine
-can be recovered in a convenient and satisfactory
that the fermentation is maintained alkaline by
the addition of various “steering” agents which
act, among Other things, to absorb the produced
carbon dioxide and thereby keep the ferment
ing mash from passing vover to the acid side. 40
manner.
-
In my
,
With the steering agents heretofore employed,
however, the fermentation liquor contained‘ not
only the amount of steering agent required to
The expression "starchy materials" refers to all
those natural plant products which contain starch
maintain a suilicient degree of alkalinity, but also
the soluble reaction products of the steering
agent and carbon dioxide. The result has been
that the fermentation liquor contains a very high
crops like potatoes, corn, oats, wheat, and also
the fruits _of trees. The starch contained in
these materials is converted in known manner
proportion of dissolved salts, which, during the
by microorganisms like yeast. In accordance‘.
concentration of the slops and the recovery of
the glycerol, continuously crystallize out.
It is accordingly a further object of the present
invention to provide a fermentation process for
hydrolyzed starchy materials wherein the nor
as the major constituent.
This includes farm
intosoluble carbohydrates which are fermented
with the ‘invention, carbohydrate solutions pro- "
50 duced in this way are subjected to a fermenta
tion in the presence of controlled amounts of cal-.
cium hydroxide. The calcium hydroxide-is add
.ed continuously or discontinuousiy during the pe
mally soluble polysaccharides and proteins and
riod of fermentation at such rates as to main- '
protein-like substances are, during the course of 65 tain an alkaline reaction throughout, the pH value
2,413,699
,4
3
of the solution being preferably kept within a
range of about 7.5 to about 8.9. The reactions
which occur are of a complex nature, involving
the influence of the dissolved portion of the cal
cium hydroxide on the interplay of the enzymes
which are responsible for the fermentation, the '
reaction of the calcium hydroxide with any acet
. aldehyde formed in the modi?ed course of the
- total sugar remaining in the mash at given hours
(solid line curve A), while the amounts of cal
cium hydroxide added in discontinuous quantities
over the same period are shown by the points B,
the dotted line C indicating in a general way the
, gradually falling requirements or, calcium hy
droxide.
.
.
The following example illustrates a, typical fer
mentation procedure in accordance with the in
fermentation, the binding of carbon dioxide, ?rst
by adsorption and subsequently by a neutraliz 10 vention, but it will be understood that the inven
tion is not restricted thereto:
ing reaction with the calcium hydroxide, and, in
Eframple.-,-973 grams of total reducing sugar
addition, the formation of insoluble compounds
- in the form of an 11.6% solution are produced by
with polysaccharides and proteins. These latter
an acid hydrolysis of wheat flour. The fermen
include chemical combinations of calcium hy
droxide with these organic substances, and com 15 tation is started by adding yeast and bringing
the temperature up to about 30° C. After the
binations held together by forces of adsorption
fermentation has proceeded for a short time and
which render polysaccharides and proteins sub
47 grams of sugar are fermented under ordinary
stantially insoluble under the conditionsexist
conditions, the addition of the calcium hydroxide
ing in the fermenting liquor. After the period of
fermentation is over, the insoluble matter is re 20 slurry with mechanical stirring of the solution is
begun. 567 grams of calcium hydroxide in the
moved by one of thelknown methods, for exam
form of a 45% slurry are added over the fer
ple, by ?ltering or centrifuging. Usually, the in
menting period of about 24 hours while the tem
soluble matter, comprising large amounts of the
perature is kept at 30°—34° C. and the pH value
calcium carbonate and yeast, is in a form in which
it can easily be separated from the solution. The 25 between 8.1 and 8.6. The yeast throughout this
alkaline fermentation remains uncontaminated
solution contains the various organic products of
and in a. healthy condition; in fact, its quantity
the fermentation, including alcohol, aldehyde,
increases. .Of the total of 703.5 grams of sugars
acetic acid in the form of calcium acetate and
converted, 50 grams are used to produce new yeast
the glycerine,‘which are recovered from the so
and from the rest, 261 grams of alcohol and 98
lution after it has been slightly. acidi?ed, for ex
grams of glycerine are. formed. After the reample to a pH value of between about 3 and 5.
moval of vthe alcohol, and preferably after ?rst
The slight acidi?cation of the solution promotes
acidifying the solution to a pH value of about
the recovery of the glycerine, and tends to reduce
further difficulties arising through secondary re
3 to 5, the glycerine is recovered from the residue
actions and foaming on distillation. The cal 35 in the conventional manner.
cium hydroxide can be added in the form of a
I claim:
dry powder; it is preferable, however, to prepare
1. Process for the manufacture of glycerine by
'
a slurry of calcium hydroxide in water and reg
fermentation of sacchari?ed. starchy‘ materials,
which comprises fermenting a solution of such
ulate its flow from the storage container into the
fermenting liquor. The fermenting mash is pref 40 sacchari?ed materials-which contains dissolved
erably agitated in any suitable manner.
'
>
polysaccharides and proteins, adding calcium hy
The recovery from solution of the glycerine
droxide to the fermenting liquor in such quan
produced according to this invention is as e?icient
titles and at such rates as to maintain an alka
‘ line reaction during the fermentation correspond
as when puri?ed sugars are used as the raw ma
terial instead of the starchynatural materials
herein employed. The insoluble material which
is obtained by the interaction of the calcium hy
droxide with the products of-the fermentation has
ing to a pH range of about 7.5 to about 8.9,
whereby insoluble calcium compounds of the poly
saccharides and proteins are simultaneously
formed, removing the insoluble matter from the
value not only as a neutralizing agent because of
fermented liquor, and recovering the glycerine
its content of calcium carbonate, but also as a 50 from the so clari?ed solution,
source of organic materials, especially non-fer
2. Process for the manufacture of glycerine by
mentable carbohydrates. These are present in
fermentation of sacchari?ed starchylmaterials,
the form of combined polymeric sugars which can
- which comprises fermenting a solution of such
be separated from their accompanying inorganic
sacchari?ed materials which contains dissolved
materials by acidi?cation and then hydrolyzed 55 polysaccharides and proteins, adding a slurry of
calcium hydroxide in water to the fermenting
to convert them into fermentable monomeric
liquor in such quantities and at such rates ,as to
The amount of calcium ‘hydroxide which is
maintain an alkaline reaction during the fermen
necessary to maintain the alkaline reaction at
tation corresponding to a pH-range of about 7.5
the desired level is, in general, of the order of that 60 to about 8.9, whereby insoluble calcium com
quantity which can be calculated as equivalent
pounds of the polysaccharides and proteins are
to the amount of carbon dioxide developed during
simultaneously formed, removing the insoluble
a completely alcoholic fermentation of the car
matter from the fermented liquor, and recover
bohydrates in the solution.
ing the glycerine from the so clari?ed solution.
The period of fermentation is considerably
3. Process for the manufacture of glycerine by
shorter than in the known alkaline fermenta
fermentation of sacchari?ed starchy materials,
tions. According to this invention, 20 to 28 hours
which comprises fermenting a solution of such
are required for 100% complete conversion by
sacchari?ed materials which contains dissolved
fermentation by the batch method. The amounts
polysaccharides and proteins, adding calcium hy
of calcium hydroxide (added to the ferment 70 droxide to the fermenting liquor in such quan
ing mash) during this period depend upon the
titles and at such rates as to maintain an alka
rate of the fermentation as will appear from the
line reaction during the fermentation correspond
attached graph (Figure 1) illustrating average
ing to a pH range ‘of about 7.5 to about 8.9 where
conditions. In this graph, the rate of the fer
by insoluble calcium compounds of the polysac
form.
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'
mentation is shown by the plot of the amount of
charides and proteins are simultaneously formed,
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2,413,699
6
removing the insoluble matter from the fermented
liquor, acidifying the so clari?ed solution to bring
the pH value to between 3 and 5, and recovering
the glycerine from the acidi?ed solution by dis
tilling the same.
‘ fermentation of sugar solutions containing dis-
solved unfermentable polysaccharides and pro
tein-like substances, ‘which comprises subjecting
the solution to the fermenting action of yeast
31
I
while maintaining the solution alkaline within a
pH range of aboutt'l.5 to about 8.9 by‘ the addi
tion of calcium hydroxide to the fermenting liquor
whereby insoluble calcium compounds of the poly
4. Process for the manufacture of glycerine by
‘fermentation of sacchari?ed' starchy materials,
which comprises fermenting a solution of such
saccharides and protein-like substances are
sacchari?ed materials which contains dissolved
disaccharides and proteins, adding \to the fer 10 simultaneously formed, removing the insoluble
matter from the fermented liquor, and recover
menting liquor approximately the amount of cal
ing the glycerine from the so clari?ed solution.
cium hydroxide equivalent to the amount of 002
'7. Process for the manufacture of glycerine by’
fermentation of sugar solutions containing dis_
as to maintain an alkaline reaction during the 15 solved unfermentable polysaccharides and pro
tein-like substances, which comprises subjecting
I fermentation corresponding to a pH range of
the solution to the fermenting action of yeast while
about 7.5 to about 8.9, whereby insoluble calcium
maintaining the solution alkaline within a pH
compounds of the polysaccharides and proteins
range of about 7.5 to about 8.9 by the addition of
are simultaneously formed, removing the in
soluble matter from the fermented liquor, acidi- _ calcium hydroxide to the fermenting liquor where
by insoluble calcium compounds of the polysac
fying the so clari?ed solution to bring the pH
charides and protein-like substances are simul
value to between 3 and 5, and recovering the
taneously formed, removing the insoluble matter
glycerine from the acidi?ed solution by distilling
from the fermented liquor, acidifying the so_clari
the same.
fled ?ltrate to a pH value of about 3 to 5, and
5. Process for the manufacture of glycerine by
thereafter distilling the liquor for the recovery
fermentation of sacchari?ed starchy materials,
to be expected from the complete alcoholic fer
mentation of the carbohydrates and at such rate
which comprises fermenting a solution of such '
sacchari?ed materials which contains dissolved
polysaccharides and proteins, adding to the fer
menting liquor approximately the amount of cal
cium hydroxide equivalent to the amount of C02
to be expected from the complete alcoholic fer
mentation of the carbohydrates during a period
of glycerine.
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8. Process for the manufacture of glycerine by
fermentation of sugar solutions containing also
30 dissolved unfermentable polysaccharides and
of about 24 hours and at such rate as to maintain‘
an alkaline reaction during the fermentation‘ 35
corresponding to a pH range of about 7.5 to about
8.9, whereby insoluble calcium compounds of the
polysaccharides and proteins are simultaneously
protein-like substances, which comprises subject
ing the solution to the fermenting action of yeast
and, after fermentation has started, adding cal
cium hydroxide to the fermentingliquor to main
tain the solution alkaline within a pH range of
about 7.5 to about 8.9, whereby insoluble calcium
‘compounds of the polysaccharides and protein
like substances are simultaneously formed, remov
ing the insoluble matter from the fermented
fermented liquor, acidifying the so clari?ed solu 40 liquor, acidifying the so clari?ed ?ltrate to a pH
value of about 3 to 5, and thereafter distilling the
tion to bring the pH value tovbetween 3 and 5, and recovering the glycerine from the acidi?ed ' liquor for the recovery of glycerine.
solution by distilling the same.
ARTHUR L. SCI-IADE.
6. Process for the manufacture of glycerine by
formed, removing the insoluble matter from the
,
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