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Патент USA US2132250

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2,132,250
Patented’ Oct. 4, 1938
UNITED STATES ‘PATENT OFFICE '
2,132,250
MANUFACTURE OF ETHYL ALCOHOL FROM
'
INDIAN CORN
TheodoreB. Wagner, New York, N. Y.
, No Drawing. Application March. as, 1934,
Serial No. 717,834
,
'7 claims. (on. ‘195-16)
This invention relates to improvements in the
manufacture of ethyl alcohol from Indian corn
and, more'particularly, to a process of produc
ing a high quality ethyl alcohol substantially
free from impurities.
it is well known that in‘ the production of
ethyl alcohol from corn certain impurities are
imparted to the alcohol, suchas fusel oil and
ester-like derivatives of fatty acids. The former
ill originates in the amino-acids of the corn, which
are natural constituents thereof; the latter are
derived from the oil, likewise naturally contained
in corn, and are formed through catalytic and
' enzymic processes referred to hereinafter. These
impurities are carried over with the alcohol
250
while the alcohol is being separated-from the
fermented mash by distillation. Various at
tempts have been ‘made to overcome the ,disad
vantages of prior processes and to prevent the
presence of these impurities in the ?nished al
cohol, but, as far as I am aware, prior attempts
have been limited to eliminate the impurities,
formed during the fermentation of the mash,
either by high recti?cation of the alcohol or by a
25 treatment thereof with chemical agents.
An object of my invention is to keep out of the
mash those constituents oi’ corn, which are the
source of the impurities in the ?nished alcohol
and I have discovered a process which accom
30 plishes the object.
It is also an, object of the invention to provide
a process, which can be carried out on an. indus
trial scale and with a high degree of e?iciency.
It is also within the contemplation of the
35 invention to provide a process, which can be
carried into practice with simple and standard
apparatus and which not only produces alcohol
of high purity but enhances the value of the by
products obtained in the manufacture of alcohol
40 from corn.
Other objects and advantages of the invention
will become apparent from the following de
scription of a preferred procedure of carrying
vthe invention into practice.
45
Shelled corn is conveyed to suitable tanks and
immersed completely in water, at an elevated
temperature, for a period of preferably from
about 40 to about 60 hours. In practice I prefer
to maintain the temperature of the water at about ‘
50 115° F. to about 125° F., although a higher tem
perature may at times be advisable. When
higher temperatures are used care must be taken
that the temperatures do not rise too high with
resulting gelatinization of_ the starch of the corn.
55 Throughout the immersion period, it is preferred
to leach the corn by keeping the water in circula
tion. by any suitable means. This circulation
serves not only to remove impurities including
amino-acids, but also favorably conditions the‘
corn for the separation of the germs as more
fully described hereinafter. In the foregoing
leaching, I prefer to employ about eight gallons
of water to each bushel of corn and to dissolve
a small quantity of sulfur dioxide in the water
before the immersion of the corn therein so as to to
guard against a decomposition of the corn.
At the conclusion of the aforesaid operation, I
withdraw the water from the ‘corn and apply
to the corn one or more washings with water in
order to free the corn from water soluble sub- 15
stances, especially the amino-acids,‘ which, as
above stated, lead to the formation of fusel oily
and to its presence in the ?nished alcohol. In
practice I prefer to subject the corn to a double
and even triple washing with fresh water. , For 20
gauging the emcacy of these washing operations
in leaching the amino-acids from the com, I use
the Abderhalden “ninhydrine" test. The inten
sity of the color reaction serves as an index of the
degree oi’ elimination achieved. It the test re- 25
suits negatively, the complete removal of the
amino-acids is indicated; if positively, washing ‘
may be continued until the desired degree is
reached.
The washed corn is next delivered to attrition 30
or “cracking” mills. The plates of the cracking
mills are so distanced that the mills, with the aid
of water, do not actually grind, but merely
“crack” the corn. The cracked corn, together
with a Suitable amount of “starch milk”, is con- 35 »
veyed to suitable vats, preferably of semi-cylin
drical shape and of adequate length, width and
height, say 10 feet long, by 3 feet wide and 5 feet
high, in which the separation of the oil bearing
germs takes place. The separation of the germs 40
from the remainder of the corn is rendered pose
sible by the difference in speci?c gravity between
the oil bearing germs and the starch milk used
as the separating medium. The starch milk is
preferably made up from starch and water, so 45
as to have a speci?c gravity corresponding to
about 10-120 Baumé, which causes the germs to
rise. to the surface of the starch milk, together
with a portion of the hulls, whereas the re
mainder of the corn (i. e., a mixture of coarse 50
starch particles, of starch suspended in water,
of the gluten and’ the balance of the hulls) col
lects at the bottom of the vats and iscarrled
oif by a suitable conveying device.
The vats are
arranged-in such manner that the inlet at the 56
2
2,132,200’
top is at a higher level than the outlet for the
germs and thus the latter are carried off from the
surface of the contents of the vats in a continu
ous flow, together with a portion of the starch
milk.
For the purpose of obtaining ethyl alcohol of
high purity, which necessitates freeing the corn
not only‘ from amino-acids, but from oil and
fatty acids as well, I have found it advanta
geous to submit the cracked corn, discharged
through the bottom outlet of the germ separating
vats, to a second and even third separation, i. e.,
I pass it again through the cracking mills or
through the germ separating vats, or both, and,
15 if advisable, repeat the operation a third time.
I have observed that the cracked corn, after
leaving the ?rst separating vat, frequently con
tains a number of germs which escaped libera-r
tion during the ?rst separation and these, I have
20 further observed, can be recovered by a repeti
the recti?cation is greatly facilitated with a ?nal
product of prime quality as the result.
The residual portion of the mash I collect and
wash, preferably in a ?lter press, and then de
liver‘it to an initial dryer, of any suitable design,
in which the moisture content is reduced to about
40%, whereupon I impregnate the semi-dry
residue with the extract of the soluble constitu
ents of corn as obtained during the immersion
of the corn in water. When drained from the
steeping tanks, this extract usually has a speci?c
gravity corresponding to about 5-6“ Baumé. I
prefer to concentrate it in vacuo to about 23°
Baumé, in which state of concentration it has the
consistency of a light bodied syrup, and I incor 15
porate this syrup with the aforesaid semi-dry
residue and thereupon deliver the mixture to a
second dryer, in which the moisture of the mix
tion of the cracking and separating procedure.
When applying the second and third separations,
ture is reduced to approximately 10%. After
grinding and screening, it is ready for the market. 20
It is characterized by a high content of nitrog
enous substances, especially amino-acids, free
I have found it preferable to vary the density of
the starch milk from that employed during the
25 ?rst separation, making it lighter or heavier, as
may best suit conditions. The collected germs
are transferred to reels in which they are thor
oughly washed with water and thereby freed
from adhering starch, which is collected sepa
30 rately and is ultimately delivered to the “cook
ers", referred to hereinafter. The washed germs
are subsequently dried in steam drums and are
?nally delivered to the oil extractors which serve
to expel the oil, known at this stage as crude
35 corn oil. The residual portion may be marketed
dom from starch and a nearly complete absence
of free fatty acids and ether soluble substances.
' While heretofore the dried residue, obtained in 25
the manufacture of ethyl alcohol from corn, was
used exclusively as a concentrated animal feed
ing stuff, the residue obtained by my new method,
as described hereinabove, lends itself to culinary
purposes and is especially well suited to a nutri 30
tional enrichment of cereal and other foods in
tended for human consumption.
It will be noted that whereas under the old
method the conditioning of the corn, prior to
mashing, is effected by milling the corn in a dry 35
as germ oil meal or it may be mixed with the
vresidual portion of the “mash”, or it may be de
livered to the “cooker”, both “mash” and
“cooker” being more fully described hereinafter.
By following the foregoing procedure, it is
40
possible to obtain a yield of crude corn oil which
is substantially at the rate of one and one-half
pound per bushel of corn. It is to be noted that
this yield is at least double that obtained here
- tofore in the manufacture of ethyl alcohol from
corn degerminated in a dry state.
The degerminated corn, discharged at the bot
tom outlet of the germ separating vats, so-called
“separators”, represents a mixture of starch,
gluten, hulls and water. This mixture, which is
50 substantially free from water and ether soluble
substances, is next delivered to an apparatus
known as a “cooker”, without further processing,
though a grinding in burr mills mayv at times
state, my improvement calls for the complete
immersion of the corn in water, and even after
the water used during the immersion, is with
drawn from the com, the further processing of
the corn is carried on in the presence of large 40
quantities of water.
As a result of my improved method of manu
facture, the distillate, i. e., the ethyl alcohol ob
tained from the fermented mash, is of a high
quality and since the ?rst and last runs of the 45
distillation, the so-called “heads” and “tails”,
are materially reduced in amount, a correspond
ingly increased yield of pure alcohol is obtained.
Although it is not likely that anyone, skilled in
the art, will confuse my new method, as above 50
described, with the process customarily employed
in present day manufacture of alcohol from
corn, I recapitulate its essential differentiating
features as follows: the immersion of the corn
in water, followed by processing in a wet state; 55
be advantageous. In the cooker, ?rst liquefac
the removal of the soluble constituents of the
tion and then sacchari?cation of the starch of corn, especially amino-acids; the recovery of the
the corn are effected through the conjoint action soluble constituents of the corn in the form of a
of malt, heat and water. The charge in the syrup; the substantially complete removal of the
cooker is known as the “mash”. After cooking oil bearing germs of the com; the recovery of 60
the oil of corn; the substantial absence of higher
60 and subsequently cooling the mash; it is trans
ferred to vats in which the fermentation i. e.,
the conversion into alcoholis carried on at a
suitable temperature. For instance, a tempera
ture of about 65-80“ F. may be used after inocu
lation of the mash with a suitable fermentating
medium, such as “distiller’s seed yeast.”- The
alcohols, as derived from corn, in the alcohol ob
tained after the distillation of the fermented
mash; ?nally, the increased yield of prime ethyl
alcohol, due to the substantial absence of higher 65
alcohols.
I claim:
fermentation is usually completed within about
'72 hours. ‘Upon conclusion of the fermentation,
1. The manufacture of substantially pure ethyl
alcohol practically devoid of fusel oil from Indian
the mash is conveyed to distilling and re-distilling
apparatus of conventional types, which effect the
separation of ethyl alcohol from the water and
corn which comprises leaching Indian corn with 70
hot water containing sulfur dioxide to dissolve
water soluble substances and amino acids, wash
ing the thus-leached corn with water to free
it from water-soluble substances including amino
acids, subjecting the wash waters to the Abder 75
other ingredients of the mash. Because of the
absence in the raw alcohol of the impurities which
hitherto have always contaminated the alcohol,
2,122,250
halden “ninhydrine” test to determine the pres
ence of amino acids, continuing the said wash
ing with fresh water until said test gives negative
results to produce leached corn freed from amino
acids, cracking the leached corn to produce a
mass containing cracked corn and oil bearing
‘germs, separating the said germs from said
cracked
corn,
subjecting ‘ said
degerminated
cracked corn freed from amino acids and con
10 taining hulls to the action of heat in the presence
of water and a small amount of malt to liquefy
3
water soluble substances and amino acids, the
said hot-water being used in the amount of
about 8 gallons to about one bushel of corn, wash
ing the thus-leached corn with water to free it
from water-soluble substances including amino
acids, subjecting the wash waters. to the Abder
halden “ninhydrine" test to determine the pres
ence, of amino acids, continuing the said wash
ing with fresh water until said test gives nega-’
tive results to produce leached corn freed from 10
amino acids, cracking the leached corn to pro
and then to‘ saccharify the same, cooling the duce a mass containing cracked corn and oil
liquefied and sacchari?ed mass, fermenting the ..bearing germs, separating the said germs from
said cooled mass at about 65° F. to about 80° F. said cracked corn, subjecting said degerminated
15 in the presence of "distiller’s seed yeast” to pro
duce ethyl alcohol, and distilling the said fer
‘ mented mass to obtain substantially pure ethyl
20
alcohol practically devoid of fusel oil.
2. The manufacture of substantially pure ethyl
alcohol practically devoid of fusel oil from Indian
corn which comprises leaching Indian corn at
about 115° F. to about 125° F. with hot water
containing sulfur dioxide, washing ' the thus
leached corn with water to free it from water
25 soluble substances including amino acids, sub
jecting the wash waters to the Abderhalden
“ninhydrine" test to determine the presence of
amino acids,- continuing the said washing with
fresh water until said test gives negative re
30 sults to produce-leached corn feed from amino
acids, cracking the leached corn to procduce a
mass containing cracked corn and oil bearing
germs, separating the said germs from said
cracked corn, subjecting said degerminated
35 cracked corn freed from amino acids to the action
of heat in the presence of water and a ‘small
amount of malt to liquefy and then to saccharify
the» same, cooling the lique?ed and sacchari?ed
mass, fermenting the said cooled mass at about
40 65° F. to’ about 80° F. in the presence of
“distiller’s seed yeast" to produce ethyl alcohol,
and distilling the said fermented mass to ob
tain substantially pure ethyl alcohol practically
devoid of fusel oil.
45
a
-
3. The manufacture of substantially pure ethyl
alcohol practically devoid of fusel oil from Indian
corn which comprises leaching Indian corn at
about 115° F. to about 125° F. with hot water,
containing sulfur dioxide, for about 40 to about
60 hours to dissolve water soluble substances
.and amino acids, washing the thus-leached corn
with water to free it from water-soluble‘ sub
stances including amino acids, subjecting the
cracked corn freed from amino ‘acids to the action 15
of heatv in the presence of water and a small
amount of malt to liquefy and then to saccharify
the same, cooling the lique?ed and sacchari?ed
mass, fermenting the said cooled mass at about
65° F. to about 80° F. in the presence of “dis 20
tiller’s seed yeast" toproduce ethyl alcohol, and
distilling the said fermented mass to obtain
substantially pure ethyl alcoholpractically de
void of fusel oil.
5. The manufacture of substantially pure 25
ethyl alcohol practically devoid of fusel oil from
Indian corn which comprises leaching Indian
corn with hot water, containing sulfur dioxide to
dissolve water soluble substances and amino acids,
washing the thus-leached corn with water to free 30
it from water-soluble substances including amino
acids, subjecting the wash waters to the Abder
halden "ninhydrine” test to determine the pres
ence of amino acids, continuing the said wash
ing with fresh water until said test gives negative 35
results to produce leached corn freed from amino
acids, cracking in the presence of water the
leached com to produce a mass containing
cracked corn and oil bearing germs, separating
the said germs from said cracked corn, subject 40
ing said degerminated cracked corn freed from
amino acids to the action of heat in the presence
of water and a small amount of malt to liquefy
and then to saccharify the same, cooling the
lique?ed and sacchari?ed mass, fermenting the 45
said cooled mass at about 65° F. to about 80° F.
in the presence of "distiller’s seed yeast” to pro¢
duce ethyl alcohol, and distilling the said fer
mented mass to obtain substantially pure ethyl
alcohol practically devoid of fusel oil.
50
6. The manufacture of substantially ethyl al
cohol practically devoid of fusel oil from Indian
corn which comprises leaching Indian corn with
wash waters to the Abderhalden “ninhydrine” hot water containing sulfurdioxide to dissolve ,
test to determine the presence of amino acids, Water soluble substances and amino acids, wash
continuing the said washing with fresh water ' ing the thus-leached corn‘ with water to free it 55
until said test_gives negative results to produce from water-soluble substances including amino
leached corn freed from amino acids, cracking acids. subjecting the wash waters to the Abder
the leached corn' to produce a, mass containing halden “ninhydrine" test to determine the pres
60 cracked corn and oil bearing germs, separating
ence of amino acids, continuing the said wash 60
the said germs from said cracked corn, subject
ing with fresh water until said test gives 'nega-_
ing said degerminated cracked corn freed from tive results to produce leached corn freed from
amino acids to the action of heat in the presence amino acids, cracking the leached corn to pro
of water and a small amount of malt to liquefy duce a mass containing cracked corn having av
65 and then to saccharify the same, cooling the
specific gravity of about 10 to about 12° Baumé 65
lique?ed and saccharifled mass, fermenting the and oil bearing germs, separating the said germs
said cooled mass at about 65° F‘. to about 80° F. from said cracked corn, subjecting said degermii
in the presence of “distiller’s seed yeast” to
nated crackedcorn freed from amino acids to
produce ethyl alcohol, and distilling the said the action of heat'in the presence of water and
70 fermented mass to obtain substantially pure ethyl a small amount of malt to liquefy and then to 70
alcohol practically devoid of fusel oil.
_ saccharify the same, cooling the lique?ed and
,4. The manufacture of substantially pure ethyl sacchari?ed mass, fermenting the said cooled
alcohol practically devoid of fusel oil from Indian ' mass at about 65° F. to about 80° F. in the pres
corn which comprises leaching Indian corn with
ence of “distiller’s seed yeast” to produce ethyl
hot water containing sulfur dioxide to dissolve alcohol, and distilling the said fermented mass 76
2,132,250
to obtain substantially pure ethyl alcohol prac
tically devoid of fusel oil.
'7. The manufacture of substantially pure
ethyl alcohol practically devoid of ~fuse1 oil from
Indian corn which comprises leaching Indian
corn with hot water containing sulfur dioxide to
dissolve water soluble substances and amino acids,
washing the thus-leached corn with water to free
it from water-soluble substances including amino
10 acids, subjecting the wash waters to the Abder
halden “ninhydrine” test to determine the pres
ence of amino acids, continuing the said washing
with fresh water until said test gives negative
results to produce leached corn freed from amino
15 acids, cracking the leached corn to produce a
mass containing cracked corn and oil bearing
germs, separating the said germs from said
cracked corn, subjecting said degerminated
cracked corn ireed from amino acids to the ac
tion of heat in the presence of water and a small
amount of malt to liquefy and then to saccharity
the same, cooling the lique?ed and sacchari?ed
mass, fermenting the said cooled mass at about
65° F. to about 80° F. in the presence of "dis
tiller’s seed yeast” for about 72 hours to pro 10
duce ethv alcohol, and distilling the said fer
mented mass to obtain substantially pure ethyl
alcohol practically devoid of fusel oil.
THEODORE B. WAGNER.
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