DECEMBER, 1940 INDUSTRIAL AND ENGINEERING CHEMISTRY 1549

American users of a protein-base fiber will doubtless de- tory fiber must go into a textile mill, be blended with other
mand a strength capable of withstanding reasonable carding, fibers, and withstand all the operations common to a textile
combing, and spinning operation without help from other plant without requiring any change in operating conditions.
fibers. They will require dyeing properties similar to wool, When, and if, a casein-base fiber is produced and offered to
under the same conditions of dyeing, because casein fiber and our domestic trade, which meets the above requirements, it
wool will be frequently mixed. Felting properties should be will doubtless fmd a successful use in many classes of textile
good in mixtures with feltable materials. The product must goods. In addition, such a fiber will have many properties
have a permanency which will avoid any breakdown by bac- unique to itself and, without supplanting or interfering with
teria, mold, etc. It must withstand all common cleansing the use of any present textile fibers, will add materially to the
agents under normal conditions of use. In general, a satisfac- versatility of the textile industry.

Soybean Protein Fibers

Experimental Production
R. A. BOYER, Ford Motor Company, Dearborn, Mich.

Production of fiber from soybean protein is de- is fast becoming one of our most important vegetable oils, is
scribed. Difficulties encountered in obtaining recovered in the first step of the fiber production.
uniform protein necessitate strict control of the
variety of the soybeans and thorough chemical Production of Fiber from Soybeans
analysis and fertilization of the soil on which they
OF OIL. The continuous solvent extraction
EXTRACTION
are grown. When good protein is used, spinning
solutions containing 20 per cent protein can be
method is used to extract the oil. The crushed beans are
obtained. Soybean fiber as made at present has
washed countercurrently with hexane which removes the oil.
about 80 per cent the strength of wool, has more
The resulting oil-free meal is passed through a steam-jacketed
elongation both wet and dry, and does not wet so
pipe for removal of the solvent. Although the Ford extrac-
easily as wool or casein fiber. It does not promote
tion equipment is different, the whole operation is standard
mold growth so readily as casein fiber. The fiber
in the soybean industry with the exception that meal pre-
blends well with wool and cotton and has been
pared for fiber work is treated at much lower temperatures
processed satisfactorily on both cotton and worsted
than meal prepared for cattle food.
EXTRACTION OF PROTEIN FROM OIL-FREE MEAL. This is
textile equipment. Plans are being made for a
pilot plant capable of producing 1000 pounds per
a critical and important part of the fiber preparation. Al-
day of soybean fiber.
though protein extraction is a relatively simple operation,
extreme care must be exercised in order to produce uniform
batches. There are many ways of extracting protein, some
of which are closely guarded secrets. The indications are that
YNTHETIC fiber production has been one of the most the simpler methods will be the most satisfactory. One

S active and fertile fields for chemical research during

the past twenty years. The tremendous growth of the
rayon industry has stimulated the interest in work along this
method is to treat carefully sized oil-free meal with a weakly
alkaline solvent, such as 0.1 per cent sodium sulfite solution,
for a half hour. The resulting solution is clarified either by
line, not only of textile chemists but of those employed in filtering or centrifuging. The protein in the solution is precipi-
unrelated fields. Until recent years the greater part of the tated with an acid, and the resulting curd is washed and dried.
work was devoted to production and improvement of cellu- Because of the discoloration of protein by iron, each one of
lose fibers such as viscose, cuprammonium, and acetate. I n these steps must be carried out in stainless steel or glass
1936, however, Ferretti in Italy published his work on a new lined equipment (Figure 1). The pH must be checked and
type of protein fiber produced from milk casein. This fiber controlled constantly. For instance, no two batches of soy-
called lanital achieved a reputation commercially as a wool bean meal will have the same pH when treated with the same
substitute because of its chemical and physical similarity amount of sodium hydroxide under similar conditions. Ac-
to wool. cordingly the alkali is adjusted to bring each batch to the
The success of lanital inspired fiber research on a great many same pH. Clarifying an alkaline solution of protein setis-
other proteins, among them, fish protein, regenerated silk, factorily is a difficult chemical engineering problem. At pres-
peanut, corn zein, and soybean. The Ford research chemists ent stainless steel centrifuges with automatic unloading de-
had several years background of soybean research in 1937 vices are being used (Figure l). However much more work
and undertook the development of a fiber from soybean pro- remains to be done on this point. Precipitation must be
tein a t that time. The soybean in many ways is an outstand- carried out a t exactly the right temperature and p H in order
ing source of protein for fiber work. Economically it is sound. to get a curd that can be satisfactorily handled during the
The supply of soybeans is large and increasing yearly. The subsequent washing and drying.
large use of soybean meal a t present is for cattle food, and In spite of all these precautions we have found variations in
this tends to keep the price stable and low. The bean is easily the proteins. We have traced these back to differences in the
grown and finds favor with the farmers. Soybean oil, which variety of the bean from which the protein was extracted.
1550 INDUSTRIAL AND ENGINEERING CHEMISTRY VOL. 32, NO, 12

There are indications also that the composition

of the soil on which the beans were growii has
a marked effect on the protein. In order to
have a uniform supply of beans for t.he fiber ex-
periments, pure strains of soyheam are heing
grown on fields that have been thoroughly
analyzed and fertilized. The crop from them
fields will be stored in special metal containerr
in order to keep to a minimum any changes
that may occur during storage. We hope by
these methods to eliminate as many variables a t
the source as possible.
PREPARATION OF SOI,UTION FOR SPINNING.
The third step in producing a fiber consists in
dissolving the protein to produce a viscous
stringy solution. It is desirable to obtain a
solntion having a high solids content. Because
of the tendency of proteins in high concentra-
tions to form a gel, i t is difficult to prepare
solutions having more than 12 per cent solids.
However, by proper control during the extrac-
tion of the protein we have succeeded in pro-
ducing solutions containing 20 per cent protein.
These solutions have excellent spinning charac-
teristics. They must, however, he aged at the
right temperature for the correct time before
the proper viscosity and stringiness are reached.
The solution a t this point should contain no
undissolved particles or air buhbles, BS the spin-
ning continuity would be affected.
SPINNING AND HARDENING. The fourth step
consists in forcing the solution through the
spinnerettes into the acid precipitating bath
and collecting the filaments on a reel or bobbin.
Although many variations in precipitating baths
are possible, they nsnally consist of sulfuric acid,
formaldehyde, and a salt such as sodium chlo-
ride or aluminum sulfate to facilitate dehydra-
tion of the filaments. Stretching is an important
part of the precipitation. The filaments are
pulled through the acid bath and over two glass
pulleys called Godet wheels (Figure 2 ) . The
second wheel revolves faster than the first and
thus exerts a stretching effect between them on
the filaments. For staple fiber work multihole
spinnerettes are used; our usual practice calls
for 500-hole spinnerettes. A spinning machine
having the flexibility required for experimental
work is quite complicated. In order to obtain
all the features wanted, we hati to design and
build our own machine.
Recently we have been working with a con-
tinuous machine that will enable us to precipi-
tate, harden, and carry out the aftertreatment
of the filaments continuously. The uniformity
of treatment obtained by the continuous machine
is a great advantage in producing fibers bc-
cause of their minute size and sensitivity. Con-
trol of stretching is important, as can be shown

F~GURE
1. (Above) STAINLESS
STEELTANKS

SEJZ-CLEANINC
CENTRIFUGES
 . (._

DECEMBER, 1940 INDUSTRIAL AND ENGINEERING CIIEMISTKY 1551

Recent refinements in processing
have produced a soybean fiber
highly resistant to carboniaing
and to boiling in dilute acid and
alkali.
The fiber has been handled on
conventional cotton and worsted
equipment. I t showsgreat promise
as a new, distinctly different fiber
eminently suited in wool blends
for use in suitings and upholstery
fabrics. The availability of the
fiber in fine deniers, with a fine
crimp and great resilience, indicates
its usefulness with cotton and spun
rayon in the development of many
new materials. Still another de-
velopment under investigation is
the use of soybean fiber with wool
in felt manufacture.
While a tremendous amount of
work remains to be done on soy-
bean fiber, we feel that the r&Tb
already obtained warrant proceed-
ing with the program as fast as
possible. Plans are now @ing
forward for the installation of a
complete pilot plant capable of
producing 1000 pounds per day of
finished fiber in the form of top
suitable for blending with fibers
FIGURE 2. EXPERIMENTAL SPINKINu MACHINE, SHoWINQFILAMENTS BEING 8PllETCHED
used in automotive upholstery. In
BETWEEN T W O (;ODET WHEELS
developing tbis fiber we think that
a definite contribution will have
by producing fibers made from the same solution with and been made not only to the textile industry and its customers,
without stretcbing. Those made without stretcbing will hut also to the suppliers of the textile industry-the farmers.
be brittle and weak; those that are stretched during the
treatment will have good elasticity and high yield points.
X-ray diffraction studies of fibers show the value of stretch-
ing. Orientation occurs when the fiber is stretched under
proper conditions, whereas indefinite x-ray patterns are ob-
tained from unstretchcd fibers.
AFTERTREATMENT AND DRYING. Aftertreatment of the
fiber consists of a relatively long immersion of the fiber in a
formaldehyde bath to set the fiber completely, cutting i t to
the desired staple length, and drying i t under controlled
humidity and temperature conditions (Figure 3). If the
fiber has been properly treated, it will be in a loose fluffy con-
dition resembling scoured wool.

Properties
The finished fiber is white to light tan in color with medium
luster; i t bas a warm soft feel, a natural crimp, and a high de-
gree of resilience.
The tensile strength of soybean fiber is about 80 per cent
8s compared to wool; its dry elongation of 40 per cent and
wet elongation of 60 per cent are much higher. The tensile
strength a t break is approximately the same dry and wet:
however, the yield point is lower on the wet fiber.
The specific gravity of soybean fiber is 1.31 measured in
water. The fiber is nearly circular and has little pigmenta-
tion. Water does not wet soybean fiber so readily as it does
casein fiber and wool. Preliminary experiments indicate that
soybean fiber is very resistant to the action of mold as com-
pared to casein fiber which is more readily attacked.
Fiber sizes range from 1.5 to 5 deniers in staple lengths of
1.5to 6 inches. It can be produced in natural color or can be F I G U ~3.~ :DRYING SOYBEAN FIBERI N I ~ I ~ M I D I T Y - ~ ~ N -
spun dyed, with or without a fixed, highly permanent crimp. TROLLED OVEN