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Патент USA US2359204

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Patented‘ Sept. Z6, 1944'
' 2,359,204
uNl'raD STATES PATENT (OFFICE.
- METHOD or PREPARING» zam SOLUTIONS
nmno'rnr mom GLUTEN
Roy. E..Coieman, Chicago, 111., assignor to Time,
Incorporated, a corporation of New York
'
No Drawing. Original application November 30.
.1942, Serial No. 467,402. Divided and this ap-'
' piication October 25,- 1943,‘ Serial No. 507,599
‘
This invention relates to methods
11 Claims. (01. 106-153)
of prepar
preferably between about 140° to about 150° F.,
ing commercially usable solutions and coating
for a short period oi’ time generally not exceed
ing about three hours. It is preferred that the
compositions of prolamines or prolamine-con
taining proteins directly from glutens, either
vextraction time be not longer than about one- '
com, wheat, barley, etc. It is particularly di 5 half to about one hour since within this time
rected to such methods which will produce solu
and at the temperatures stated, the zein in the
tions and coating compositions of the alcohol
gluten is extracted and is not deleteriously af
' soluble portion of corn gluten, of controlled so- '
lution and gelling characteristics. -
This application is a division of my copending
application, Serial No. 467,402, iiled November
30, 1942. ‘
fected.
10'
‘
The extract solution obtained as above de
scribed is now separated from the residual gluten
by'?ltration, pressing, centrifugal separation or »
in any other desirable manner and is distilled
Heretoiore, in the preparations of zein solu
or otherwise treated to remove all or some of the
tions and coating compositions,‘ including the
diluent, as desired. It may be ?ltered prelimi
substantally non-aqueous ‘rein solutions and 15 narily to the step of removing the diluent, if
coating compositions of ‘controlled solution and
necessary. The resulting residue is a solution of
gelling characteristics as described in my prior
zein or zein-containing protein in the base sol
Patent No. 2,185,110, granted December 26, 1939,
vent alone with all of the diluent from the ex- .
for example, the zein is initially isolated irom
tract solution removed, or in .the base solvent
and that portion of the diluent which has not
corn gluten and ‘thendissolved in suitable sol
vents to form the desired solutions. To isolatev
- ‘been removed.
The residual gluten, which still
zein from corn gluten as a commercially usable
contains some protein, may be freed from re-i
powder is a laborious and expensive process, in
tained solvent by washing and recoveredior' .
further use as a cattle food or for other purposes.
volving steps‘ of precipitation, settling, ?ltering,
washing and
‘ The solubility of the zein
in zein solvents and the solution ch..racteristics
such- as stability and gelling tendencies are
largely dependent upon the care exercised in
_ carrying out the steps'oi the process.
The resulting zein or zein-containing solutions
in accordance with the present invention, over a
wide range of concentrations, are stable on
, standing at temperatures of 80° F. and below
and do not-separate even when cooled to tem
In accordance ‘with the present invention I v30 peratures of 50 to 70° F. and somewhat below.
prepare solutions ofv zein or' zein-containing
proteins directly from corn gluten under condi
tions that will readily produce awideyariety oi
‘When cooled even to temperatures'as low as 10°
above zero or to zero, solutions prepared in ac
cordance with the present invention may sepa
rate and become solid: however, on heating
bility characteristics are concerned, and thereby 35 again to temperatures of from about 45° to 70°
avoid the expense and objections incident to '
F., a re-solution is eiiected, either without stir
the preliminary isolation or zein in powder form.
ring or with slight stirring, and the solutions
In carrying out the present invention, corn
return to their normal. form at the reheating
gluten, for example, .in granular ‘or powdered
temperatures. Ingeneral, these solutions are
form, is treated with .a suitable solvent mixture, 40 substantially non-gelling and have but a slight
without the establishment‘ oiap'eeial conditions ' tendency to increase in viscosity; that is,‘ to
of hydrogen ion concentration either in the sol
thicken or become heavier in body. In many
vent or‘ in the gluten,.- to extract the rein from
instances they exhibit practically no tendency
the gluten. The solvent mixture comprises a
to thicken or to gel over practical periods ofv
base solvent having a boiling point above about 45 time in the order of about 3 to 6 months and
125° (2., preferably above about 150‘ C. and a
even up to one 'year and longer. These solu
diluent or extender having a boiling point be
tions remain stable and reasonably constant in
' low about 125° C. and, preierably, or about 100°
their characteristics" during the periods neces
C. and below. The base solvent is itself a sol
sary for transportation and distribution, either
zein products in so far as properties and solu
vent for zein and the diluent maybe, and pret
erably is. also a solvent for zein. ‘ The base sol
vents and diluents in accordance. with the pres
ent invention will be defined fully hereafter.
The extraction is carried out at elevated tem- '
in bulk or inpackages, or for storage for reason
able periods of time, and hence their field of ap
,p'licability is greatly increased.
In general, in the concentration of zein orv
other prolamine in commercially usable solutions
peratures, say from about 1209' to about 170° lit, -_55 containing about 12 to [30% of protein, the
2
2,869,204
amount of base solvent necessary to obtain these
concentrations in the ?nal solutions is in and
of itself insu?lcient to give the proper relation
between solvent and gluten ,for effective extrac
tion results. If large amounts of the relatively
high boiling point base solvents are used, suill
eient to give the proper relation between solvent
and gluten, the extraction results are not sum
ciently effective and, moreover, the cost ot‘treat;
ing the extracts to obtain the desired solids con
kinds of solvents which may be used as base sol
vents in accordance with the present invention
than is-disclosed‘herein, reference is made to the
description of these solvents in‘ my prior Patent
centration is so prohibitive as to make this pro
cohol, cyclohexanol, iurfuryl alcohol, tetrahy
No, 2,185,110.
'
Examples of base solvents in accordance with
the present invention are the glycols such as di
ethylene glycol, propylene glycol, trlethylene gly
col and mixtures thereof, including mixtures
which contain ethylene glycol; diacetone alcohol:
closed chain cyclic alcohols such as benzyl ai
cedure commercially unfeasible.
The desired solvent to gluten ratio in accord
ance with the present invention is secured by
adding to the desired amount of relatively high
boiling point base solvent or mixture of base sol
drofurfuryl alcohol and mixtures of closed chain
alcohols; glycol others such as ethylene glycol
mono-methyl ether, diethylene glycol mono
methyl ether, ethylene glycol mono-ethyl ether,
diethylene glycol mono-ethyl and mixtures of
vents one or more of the so-called relatively low
glycol ethers; mixtures of two or more of the
boiling point diluent solvents. To obtain e?ec
tive extraction results, the solvent to gluten ratio
should be in the order of about 21/2 to 10 parts
by weight of the former to about 1 part by weight
foregoing enumerated base solvents; mixtures of
one or more of the foregoing base solvents with
glycerine, or other solvents or mixtures of sol
vents, providing the mixture has the required
of the latter. Due to the presence of a diluent
polar to non-polar radical balance and the re
or extender in the extracting solvent, the solvent
quired
relatively high boiling point. It is to be
to gluten ratio may be less than that which would
be required with a base solvent alone and, not 25 understood that the foregoing speci?cally men
tioned solvents or mixtures of solvents is not in
withstanding the lower solvent to gluten ratio,
tended
to- be inclusive of all the base solvents
the extraction results are generally more eilec
which may be used in accordance with the pres
.tive. The diluent solvent or extender must have
ent invention since they are merely set forth for
a lower boiling point and distillation range than
illustrative purposes.
the base solvent. It is preferred that these allDiluent solvents .
uent solvents or extenders be of substantially
lower boiling point and distillation range than
The diluent solvents or extenders in accord- the base solvent, as pointed out above.
'
.
ance with the present invention may be, suit
ably, a single solvent or a solvent mixture which
Base solvents
, The base solvents are relatively high boiling
may or may notbe a solvent for zein or other
one hand, having 53% hydroxyl and 47% hydro
within the percentage range stated. For con
venience herein I ‘term these alcoholic solvents
prolamine, as desired. It is preferred, however,
compounds or mixtures of compounds as pointed
that the diluent or extender be a solvent for zein.
out above and have asultable balance between
Thus, the extending. solvent may be one or more '
the hydrocarbon constituents or radicals present
in the solvent or solvent mixtures and the polar 4.0 of the well-known alcoholic zein solvents such as
anhydrous methanol, or constant boiling point
constituents or radicals present therein. A cer
mixtures (azeotropes) of aliphatic alcohols such
tain proportion of hydroxyl radicals in the base
as 95%-ethyl alcohol and 91% isopropyl alcohol.
solvents is required to secure solvent action.
For convenience herein I term these alcoholic
Other polar radicals such as —O— (ether oxy
gen), —Cl, —NH: and COOH appear to aid or 45 solvents "concentrated alcohol solvents.” The ‘
diluent solvents may also beone or more of the
cooperate with the —OH in securing the nec
concentrated alcohol solvents containing addi
essary conditions of polarity in the base solvents
tional
amounts of water, say from 40% to 50% in
(in which term I include mixtures oi’ base sol
anhydrous methanol or in excess of that present
vents) ,for solvent action.‘
'
The proportion of polar radicals to hydrocar 50 in the azeotropes 95% alcohol and 91% isopropyl
alcohol. Greater or lesser amounts of water than
bon or non-polar radicals which I have found to
as stated may be used; however, best results are
be desirable lies within a range which extends
obtained with the use of added amounts of water
between the limits oi! absolute methanol on the
carbon radicals, and absolute ethanol on the
_ _“aqueous alcohol mixtures."
other hand having 37% hydroxyl and 63% hy
Another class of diluent solvents in accord-.
.ance with the present invention’ comprises mix
tures of an azeotropic concentrated alcohol sol
cals. This range is approximate and may vary ‘somewhat depending on the solvent or solvent 60 vent with a non-solvent and water. Examples
of such diluents are mixtures of 95% ethyl alco
mixture used. The limits of this range are inhol
or 91% lsopropyl alcohol with dichlorethyl
dicative of solvent properties and provide a close
ene, trichlorethylene, ethyl acetate, benzene, cy
and adequate guide to‘ enable the operator, .by
clohexane, etc., and water. In‘this class 01' d'ilu
simple experimentation, to determine the re
ent solvents I, also include non-aqueous azeo
quired balance of polar and hydrocarbon radi
drocarbon radicals. The benzyl radical acts as
it it were intermediate the methyl and ethyl radi
cals in the base solvent or mixture of base 501- >
vents in accordance with the present invention.
It may be stated that the base solvents in
,-tropic mixtures of anhydrous methyl alcohol '
with hexane, cyclohexane, benzene, carbon tetra
chloride, dichlorethylene, trichlorethylene,v ace
accordance with the present invention may be
tone, methyl acetate, ethylacetate, methyl ethyl
- described in my prior Patent No. 2,185,110 which
ture, methyl alcohol, is a zein solvent.
In addition to the foregoing, wherein at least
any one of the solvents or mixture of solvents 70 ketone, etc. because one constituent of, the mix- -
has the required balance of polar and non-polar
one constituent of a diluent solvent mixture is a
radicals, anda boiling point above about 125° C.,
preferably, above about 150° C. as pointed“ out
above. For a more‘ complete description of the
1:
zein solvent, thediluent ‘solvents may be suitable
azeotropic mixtures. which are acid protein sol
3.
2,8579,204 -
vents wherein the individual constituents of the
mixture are non-solvents for zein proteins.
Thus, they may be azeotropic mixtures of water
on the one hand and dioxan or butyl alcohol on
the other. Dioxan forms with water a constant
boiling point mixture containing 80% dioxan
_ expected, and some of them may undergo changes -
(apparent insolubility, for example) , during the
diluent and water removal which affect the sol
vent characteristics of the zein and zein-contain
ing proteins in the base solvent utilized. These ‘
changes, where they take place, are not of a
boiling at 86.9” C.; and butyl alcohol forms with I permanent character and it is possible to effect
water a constant boiling point mixture contain
a, re-solution of. the zein or zein-containing pro
ing 63% butyl alcohol boiling at 92° C. They
teins in the base solvents by the addition of a
may also be suitable aqueous azeoti‘opic mix-' 10 small amount or water, say in the‘ order of from
tures which are non~solvents for zein proteins
about 1 to 3% by weight, ‘or an equivalent
such as ethyl methyl ketone and water. And
amount of- other highly hydroxylated compound,
they may also be non-aqueous azeotropic mix
such as methyl or ethyl alcohol or a mixture of "
tures of anhydrous ethylalcohol or anhydrous
such compounds.
'
isopropyl alcohol with hexane, cyclohexane, ben 15
In the preparation of usable solutions having
zene, carbon tetrachloride, dichlorethylene, tri
a. wide ?eld of applicability, I prefer that the
chlorethylene, acetone, methyl acetate, ethyl ace
tate, methyl ethyl ketone, etc.
, removal of diluent and waterbe controlled so
The diluents may also be suitable non-solvents
of low polarity characterized by the presence of
- to 3% by weight of water or an equivalent
—O—, --Cl, —NHz, —COOH groups, etc. Exam
ples of such diluents are dioxan, dichlorpentane,
ethylene dichloride, dichlorethyl ether, etc. They
. may, also be miscible hydrocarbons such as ben
as to leave in the ?nal solutions at least about 1
20. amount of other highly hydroxylaled compound,
preferably water. Where this is not possible,‘ wa
ter may be added to the ?nal solution, in the
amounts stated. While water is, in general, not
essential constituent of some of the solutions '
zene, hydrogenated naphtha, etc. Or they may 25 an
formed in accordance with the present invention,
be suitable non-solvents of high polarity such as
the solutions are generally of an improved char
anhydrous ethanol, anhydrous isopropanol or
acter when they contain small amounts of water.
The solutions may contain larger amounts of
In general, extracting solvents consisting of
water, say between 5 to 10%, or even more.
or including the aqueous alcohol mixtures are 30
As already pointed out, the type ‘or character
capable of extracting larger amounts of zein pro
of the zein-containing protein produced by the
water.
.
~
-
tein from gluten than are the extracting solvents
extraction is in no, small part dependent on the
consisting of or including a concentrated alco
character of the extraction solvents used. This
hol solvent. It has been noted that for practi
condition is particularly pronounced when the
cal extraction procedures‘, using either a concen 35 highly aqueous alcohols or the high water
trated alcohol solvent alone or an aqueous alco
hol mixture alone, approximately 21/2 parts by a
azeotropes'such as dioxan-water or n-butyl alco
hol-water mixtures are used as diluents.v Not
only‘ do these diluents e?ect the extraction of a
weight of solvent to l‘ of gluten may be used. At
this concentration, with gluten containing ap
larger amount of the ‘zein-containing protein
proximately 60% total protein, the extract solu 40 than do the more concentrated alcohols, but
~ tions of the concentrated alcohol'solvent contain‘
they also produce by their extraction a type 01"
a maximum zein protein content of approxi
' zein protein which generally produces solutions '
mately 10% whereas the extract solutions of the
having a high viscosity and pronounced colloidal
aqueous alcohol mixture solvents contain a'maxi
consistency. On the other hand the zein pro-'
mum ‘zein protein content of from about 12% to 45 tein produced with the concentrated alcohols;
about 15% and even up to 20%. In addition,’ the
and less aqueous diluents tends to produce solu
aqueous alcohol mixture solvents are capable of
tions having a lower viscosity and a lesser col
extracting a substantially larger proportion of
lcidal consistency. It is thus evident that vari
a desirable type of zein present in the protein of
ous types ofv zein protein having substantially
the gluten than are the concentrated alcohol sol— 50 di?'erent properties can be produced by proper
vents.
.
'
Zein solutions-of a desired concentration and
of a wide applicability can be obtained directly
from gluten by having in the ?nal solution as
the only solvent or as the main solvent for zein,
a relatively high boiling point solvent having the
required balance of polar and non-polar radicals
as described herein.
It is now well established
selection and composition of the diluents. -
From the'"~_foregoing it is manifest that the
nature'and properties of the ?nished solution
will be determined by the nature of the base
solvent, the amount of zein protein present in
the solution and the type or character of the
zein ‘protein extracted by the particular diluent
used. It is apparent that with the solveritand
diluent combinations possible, a wide variety of
tical usability of zein solutions are in no small 60, solutions for many uses can be produced by the
that the ‘viscosity, gelling tendencies, and prac
' part dependent upon the character of the solvent
in which the zein is dissolved.
Zein or zein-containing extract solutions con
taining any one or more of the foregoing base
methods of the present invention. '
:
Within the range of the many possible com;
binations and the methods in accordance with ,
the present invention, solutions may be pro
solvents in accordance with the present inven 05 duced which require further adjustment or
tion, may be boiled, distilled or otherwise treated
modi?cation in order to secure improved solu
to remove part or all of the diluent. It is evident
tion or desired stability and controlled gelling
that practically all 01' the diluent, including any
properties. vSuch adjustments or modi?cations
water carried from the gluten to the extract solu-'
can be readily eifected by the use of rosin, fatty .
tion, may be removed, thereby obtaining solutions 70 vacids,'compatible amines such as monoethanol
of zein or zein-containing. proteins, in the base
amine, triethanolamine, etc., amine soaps of '
solvent which, for all'pralctical purposes, are sub
rosin or fatty acids,v or by the various methods
stantially anhydrous. vSuch solutions vary wide
and materials for producing stable, controlled
ly in character, depending upon the choice of
"gelling, zein solutions described in my issued
’ solvents or solvent mixtures used, as is to be 75 ‘Patents Nos. 2,185,122; 2,246,779 and 2,298,548.
_
4-,
.
2,359,204
.
ethylene glycol and 25% of ethylene glycol mono
The addition of'suita'hle materials for, effecting
desired modification or adjustment may be made
to the extract solution before distilling of! the
ethyl ether was added to 30 parts of powdered
gluten. The procedure was as in Example 1 ex
cept that the extraction temperature was 140', I".
diluent or to the final solution. The preferable
The resulting residue was a_solution of fzein-con
taining proteins principally in the glycol and gly
procedure and materials with particular solu
tions may be readily determined by experimenta
col ether mixture.
‘ tion.
1
Example 7.-A solvent mixture containing 60
parts of a mixture consisting of 90% of 91% iso
10 propane] and 10% or water, and 40 parts of a
mixture consisting of 75% of diethylene glycol
ance with the present invention. In the exam
pics and elsewhere throughout thespeci?cation, , - and 25% of ethylene glycol monomethyl ether was
added to 30 parts of powdered gluten. The pro
the term “parts" indicates parts by weight. w '
cedure was as in Example 1 except that the ex
Example 1.—A solvent mixture containing '12
traction temperature was 140° F. The resulting
parts of anhydrous isopropyl alcohol (99%), 40
residue was a solution of the min-containing pro
parts of diethylene gylcol and 8 parts of ethyl
teins principally in the glycol and glycol ether
' ene' glycol was added to 30 parts of powdered
mixture.
gluten in a vessel. The mixture was heated to
_ Example 8.—A solvent mixture containing 60
about 160° F. and held at about that tempera
ture for about 1/2 hour with stirring to extract 20 parts of a mixture consisting of 80% of denatured
95% ethyl alcohol ("Paco") and 20% of water.
‘the zein-containing proteins from the gluten.
and 40 parts of a mixture consisting of 75% of
The mixture was then ‘forced through a ?lter to
diethylene glycol and 25% of benzyl alcohol was
separate the zein-containing extract and the
In the following examples I disclose illus
trative methods for producing zein or zein-con
taining solutions directly from gluten in accord
added to 30 parts of powdered gluten. - The pro
cedure was as in Example 1 except that the ex
traction temperature was 140° F. The resulting
residue was a solution of the zein-containing pro
extract was then slowly heated to about 250°‘ F.
and held at about that temperature with stirring
until cessation of visible boiling. The residue was
a solution of zein-containing proteins principal
teins principally in the glycol and benz'yl‘ alcohol
ly in the mixture of glycols.
In the following examples the manipulative
mixture.
'
v
’
At the cessation of boiling as referred to in
procedures were the same as those set forth in .
the examples some proportion of the lower boil
Example 1, with the exceptions hereinafter
ing constituents of the diluent originally used re
mains in the ?nal solution. The proportion there
of so remaining depends upon the iinaltemperaé
Example 2.—~A solvent lmixturecontaining 72
Q parts-of anhydrous denatured. alcohol (“Paco”), 35 ture and the boiling point curve of the mixture.
Considerable proportions'of the diluent or of its
d0 parts of diethylene glycol and 8 [parts of
noted, and in each instance the extracts were
heated until cessation of visible boiling.
.
constituents, including water. may remain with
ethylene glycol was added to 30 parts of pow
out causing gelling of the ?nal solution in reason
able periods of time.’ This is particularly true '
dered gluten. The procedure was as in Example
1 and the resulting residue was a solution of
where the glycols are used. In this respect the
zein-containing proteins principally in the mix
ture of glycols.
. ?nal solutions show differences from solutions of
-
commercial zein containing large amounts of
Example 3.—A solvent mixture containing '72
~ water as in the prior art, apparently by reason of
parts of 91% isopropanol and 48 parts of a mix
ture consisting of 88.9% of propylene glycol and
11.1% of diethylene glycol monoethyl ether was
added to 36 parts of powdered gluten. The pro
cedure was as in Example 1 except that the ex
traction temperature was 180° F. The result
ing residue was. a solution of min-containing
proteins principally in the glycol and glycol
ether mixture.
Example 4.—A solvent mixture containing so
parts of denatured 95% alcohol (“Paco”). and
to parts of a mixture consisting of ‘75% of di
ethylene glycol and 25% benzyl alcohol was
added to as parts of powdered vgluten. The
procedure was as in Example 1 except that the
extraction temperature was 140° F. The result
ing residue was a solution of zein-containing
' proteins principally in the diethylene glycol and
benzyl alcohol mixture.
Example 5.-A solvent mixture containing 60
parts of anhydrous synthetic methanol and 40
parts of a solvent mixture consisting of 75%
some changes in the character or structure of
the zein-containing proteins of the corn gluten
45
‘
50
taking place in the process of the present inven
tion, the nature of which changes is not as yet
understood.
In general and in?uenced by the type and
amount of zein protein present, the solutions pre
pared as described above and the coating com
positions prepared therefrom have the properties,
particularly when heated, of being able to "give
up” their solvent or solvents readily, and when
applied to any surface they quickly and readily
form‘ tough, ?exible, non-tacky, hard and 8811-.
: erally transparent coatings even when retaining
some solvent. The coatings formed by these sein
~containing solutions and coating compositions are
very strong and have adherent properties. In
60 these-solutions. and coating compositions the film
forming properties thereof can be built up to pro
duce films of great toughness, ?exibility, hard
ness and gloss. Under normal temperature con
of diethylene glycol and 25% of ethylene 8111200] 66 ditions, many of the zein-containing solutions or
coating compositions. will produce non-blushing
monoethyl ether was added to to parts of pow
dered gluten. The procedure was as in Example
1 except that the extraction temperature was
140° F. The resulting residue was a solution of
the hem-containing proteins principally in the
diethylene glycol and glycol ether mixture.
coatings on drying, without the aid of supple
meritary anti-blushing agents as in the prior art.
The coating compositions prepared from the above solutions may be modified and used as fully .
described in. the aforementioned application, Be
ria-l No. 467,402.
Example 6.-—A solvent mixture containing 69
While my invention has been described in con
parts of a mixture consisting oi 80% or denatured
nection with certain speci?c examples, it is, of
%% ethyl alcohol (“Paco") and 20% of water,
to parts of a mixture consisting of 75% oi di- my course, obvious it' is not to be construed as lim
~ 2,359,204
ited to these examples or to‘ the details of the
'
to form the aforesaid solution.
4. The method of preparing directly from
gluten a solution of zein-containing proteins in a
mixture of solvents comprising as essential sol
vent constituents for the zein-containing pro
'
In the claims, the expression “an elevated tem
perature in the order of about 120° F. to about
170° F." is not to be construed as a precise critical '
teins, a mixture of solvents each having a boil
ing point above about 150° C. and having a pro-,
portion of polar to non-polar radicals which lies
within a' range extending between the limits of
range, but, rather, as a range of temperatures
indicative of the elevated temperature at which -
the extractions may be carried out.
I claim: '
I
'
1. The method of preparing directly from
5
substantially all of the diluent from the extract
methods set forth therein, since obvious changes
in materials, proportions and method details will
be apparent from the foregoin~
.
' the proportion of polar to non-polar radicals of’
methanoland the proportion of polar to non
gluten a solution of zein-containing proteins in a
polar radicals of ethanol, which comprises con- '
mixture of solvents comprising as essential sol
tacting gluten with a solvent mixture at an ele
vent constituents for the min-containing pro
vated temperature in the order of about 120°_
teins, a mixture of solvents each having a boil
F. to about 170° F. to extract zein-containing
ing point above about 125° C. and having a proproteins from the gluten, said solvent mixture‘
portion of polar to non-polar radicals which lies
comprising the aforesaid zein-containing pro
within a range extending between the limits of
tein solvents having boiling points above about
the proportion of polar to non-polar radicals of 20 150° C. and a miscible diluent therefor having
methanol and the proportion of polar to non
a boiling point'below about 125° 0., said diluent
polar radicals of ethanol, which comprises con
being a solvent for said zein-containing proteins,
tacting gluten with a solvent mixture at an ele
separating the extract from the residual gluten
vated temperature in the order of about 120°F'.
and removing at least part of the diluent from
to about 170° F. to extract zein-containing pro 25 the extract to form the aforesaid solution.
teins from the gluten,.said solvent mixturecom
5. The method of preparing directly‘ from
prising the aforesaid zein-oontaining protein sol
gluten a solution of zein-containing proteins in a
' vents‘having boiling points above about 125° C.
mixture-‘of solvents comprising as essential sol
and a miscible diluent therefor ‘having a" boiling
vent constituents for the zein~containing pro
point below about 125° C., separating the ex 30 teins, a mixture of solvents each having a boil
tract from the residual gluten and removing at
ing point above about 150° C. and having a pro
least part of the diluent from the extract to form _
portion of polar to non-polar radicals which lies
the aforesaid solution.
within a range extending between the limits of .
2. The method of preparing directly from glu
the proportion of polar to non-polar radicals of
ten-a solution of zein-containing proteins in a 85 methanol and the proportion’ of polar to non-polar
mixture of solvents comprising as essential sol
radicals of ethanol, which comprise contacting
vent constituents vi’or the zein-containing pro
gluten with a solvent mixture at an elevated
teins, a mixture of solvents each having a boiling
temperature in the order of about .120? F. to
point above about 150° C. and having a propor
about 170° F. to extract zein-containing pro
tion of polar to non-polar radicals which lies 40 teins from the gluten, said solvent mixture com- -.
withhi a range extending between the limits of.
prising the aforesaid zein-containing protein
the ll‘oportion of polar to non-polar radicals of
solvents having boiling points above about 150°
methanol and the proportion of polar to non
C. and a miscible diluent therefor having a boil- _
polar radicals of ethanol, which comprises con
ing point below about 100° C., said diluent being
tacting gluten with a solvent mixture at an ele 45 ‘a substantially anhydrous solvent for said zein
vated temperature in the order of about 120° F.
containing proteins, separating the extract from
toiabout 170° F. to extract zeinecontaining pro
the residual gluten and removing at least part of
teins from the gluten, said solvent mixture com
the diluent from the extract to form the afore
prising the aforesaid aein-containing protein sol
said solution.
vents having boiling points above about 150° C. 50 6. The method of preparing directly from
and a miscible diluent therefor having a boiling
gluten a solution of zein-containing proteins in
is
point below about 100° C., separating the extract
‘ from the residual gluten and removing at least
part of the diluent from the extract to form the
aforesaid solution.
'
a mixture of solvents comprising as essential '
solvent constituents for the zein-containing pro
teins, a mixture‘ of solvents each having a boiling
65 point above about 150° C. and having a propor
'3. The method of preparing directly from
tion of polar to non-polar radicals which, lies
gluten a solution of zein-containing proteins in.
within a range extending between the limits of
a mixture of solvents comprising as essential sol
vthe proportion of polar to‘non-polar radicals of
vent constituents for the zein-containing pro
methanol and the proportion of polar to non
teins, a mixture of solvents each having a boiling 60 polar radicals of ethanol, which comprises con
point above about 150° C. and having a propor
tacting gluten with a solvent mixture at an
tion of polar to non-polar radicals which lies
within a range extending between the limits of
elevated temperature in the order of about 120°
F. to‘above 170° F. to extract zein-containing
the proportion of polar to non-polar radicals of
proteins from the gluten, said solvent mixture
methanol and the proportion ofv polar to non 65 comprising the aforesaid zein-containing pro-v
- polar radicals of ethanol, which comprises con
tacting gluten with a solvent mixture at an ele
tein solvents having boiling points above about
150° C. and a miscible diluent therefor having
vated temperature ‘in the order of about 120°
a boiling point below about 125° C.,- said diluent
1''. to about ‘170° F.,_to. extract zein-containing
being an aqueous solvent for said zein-contain- '
proteins from the gluten, said solvent mixture 70 ing proteins, separating the extract from the
comprising the aforesaid zein-ccntaining protein
solvents having boiling points above about 150°
C. and a miscible diluent therefor having a boil
. ing point below about 125° C., separating the ex
tract ‘from the residual gluten and removing
residual gluten and removing at least part of the
diluent from the extract to form the aforesaid
solution.
I
'
"
7. The method of preparing directly from glu- >
75 ten a solution of zein-containing proteins in a
2,859,204 , "
I 6
mixture of solvents comprising a glycoland a
' comprising a glycol, .a glycol ether and a miscible
diluent therefor having a boiling point below
about 125° (1.,’ said diluent being an aqueous
glycol ether as essential solvent constituents for
the zein-containing proteins, . which comprises
contacting gluten with a solvent mixture at an
solvent for said zein-containing proteins. separat
i'ng'the extract from the residual gluten and re
moving, at least part of the diluent from the ex
elevated temperature in the order of about 120°
F. to about 170° F. to extract zein-containing
proteins from the gluten, said solvent mixture
tract to form the aforesaid solution.
'
. .10. The method oi! preparing directly from glu
ten a solution of zein-con‘taining proteins in a
comprising a glycol, a glycol ether and a miscible
diluent therefor'having a boiling ‘point below
of solvents comprising propylene glycol
about 125° >CI., separating the extract from the 10 mixture
and
diethylene
glycol monoethyl ether as essen
residual gluten and removing at least part of the
solventconstituents tor the zein-containing
diluent from the extract to form the aforesaid _ tial
proteins, which comprises contacting gluten with
.
a solvent mixture at an: elevated temperature in
8. The method of preparing directly from glu
the order of about 120° F. to about 170° F. to ex-‘
15
ten a solution of zein-containing proteins'inv a
tract zein-containing proteins from the gluten,
mixture of solvents comprising a glycol and a
solvent mixture comprising propylene glycol,
glycol ether as essential solvent constituents for ' said
diethylene
glycol monoethyl ether and 91%.iso-.
the zein-containing proteins, which comprises
propyl alcohol,’ separating the extract from the
contacting gluten with a solvent mixture at-an
gluten and removing at least parto! the
elevated-temperature in the order of about 120°_ 20 residual
isopropyl alcohol from the extract to form the
solution.
_
V
'
F. to about.l70° F. to extract. zein-containing
aforesaid solution-
proteins from the gluten, said solvent mixture
.
11. The methodoi preparing directly from glu
comprising a glycol, a gylcol ether and a misci
ten a solution of zein-containing proteins in a
ble ‘diluent therefor having a boiling point below
about 125° C., said diluent being a solvent for said
mixture of solvents comprising diethylene glycol -
and benzyl alcohol as essential solvent constitu
forthe rein-containing proteins, which com
from the residual gluten and removing at. least ents
prises
contacting gluten with a solvent mixture
part of the diluent from the extract to form the
at an elevatedtemperature in the order of about
aforesaid solution.
120° F. to about 170° F. to'extract zein-contain
9. The method of preparing directly from glu-l 80 ing
proteins from the gluten, said solvent mix
ten a solution of zein-containing proteins in a '
zein-containing proteins, separating the'extract
ture comprising diethylene glycol, benzyl alcohol,
95% ethyl alcohol and water, separating the ex
tract from the residual gluten and removingat
mixture of solvents comprising a 'glycol» and a
glycol ether as essential solvent constituents‘ for
the zein-containing proteins, which comprises
contacting gluten with a solvent mixture, at an
elevated temperature in the order 01' ‘about 120°
it‘. about 170° F. to extract zein-containing pro-'
teins from the gluten, said solvent mixture
as
least part of the.95% alcohol and water from the
extract'to form the aforesaid solution; .
ROY E. COLEMAN.
'
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