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D¢¢= 31, 1946»
F. w. KRESSMAN- EI'AL
2,413,326
RESINOUS MATERIAL. AND PROCESS .OF PREPARING THE SAME
Filed Jan. 5, 1942
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ATTORNEYS.
Patented Dec. 31, 1946
2,413,326 '
UNITED ‘STATES 'PATENT' OFFICE
2,413,326
RESINOUS MATERIALS AND PROCESS OF
, PREPARING THE SAME
Frederick W. Kressman and Frederick W. Kress
man. Jr., Laurel, Miss., assignors of one-half to
Continental Turpentine & Rosin Corporation,
Inc‘., Laurel, Miss., a corporation of Mississippi
1
Application January 5, 1942, Serial No. 425,700 '
9 Claims. (Cl. 260-104)
This invention relates to a resinous plastic
material and a process of preparing the same
2
shown) extending about the outside thereof for
receiving the heated vapor of a high boiling
and more particularly to a process of reacting
liquid. In this Way, the temperature of the drum
rosin with a ligno-cellulosic materia1 at an ele
and the material therein may be accurately con
vated temperature and obtaining from the re
trolled during the heating operation and the fur
action a thermo-setting plastic.
nace may be eliminated.
An object of the invention is the preparation
The container II is equipped with an inlet
of a new and improved thermo-setting plastic
opening M which receives the discharge-end of a
or resin and the development of an ‘improved ' tubular conveyor IS, the opposite end of the con
process of making the same. Another object is 10 veyor being in communication with the outlet
to provide a process for utilizing wood and other
I6 of a hopper H. The conveyor l5 preferably
ligno-cellulosic materials particularly in the form
carries a screw ?ight l8 on the shaft l9, the
of residues such as those obtained from the acid
shaft i 9 being driven by any suitable power
hydrolysis of Wood and from the extraction of
means. Preferably the screw ?ight l8 extends
wood with steam and solvents. Still another ob 15 to a point closely adjacent the inlet opening 14
ject is to provide a process for reacting ?brous
but is spaced slightly from the drum ll.
ligno-cellulosic materials such as wood ?bers or
Said drum H is equipped in the lower portion
particles of relatively low density with rosin to
thereof with a suitable outlet 24 controlled by
form a resinous material.
'
the valve 25. This outlet may be used to remove
Another object of the invention is to provide 20 from the drum the liquid product of the reaction“.v
a process for reacting ligno~cellulosic materials
In the upper portion of the drum II is an outlet
with heated rosin in varying proportions to ob
26 which permits' the escape of excess vapors
tain resinous materials of different character
from the container.
_
istics. Another object is to provide a resinous
Within the drum II is a scraper 20 which
plastic material which is thermo-setting and 25 is carried by the rotatable shaft 2|, the shaft
which may be used as a molding resin or as a
being driven by any suitable power means. The
coating resin. Yet another object is to provide
scraper 20 may be equipped, as shown, with a
a resinous plastic material which is highly re
plurality of scraper blades 21 which pass along
sistant to alkalies and acids and which is sol
the inner periphery of the drum I I.
uble in only a limited number of organic solvents. 30
In the operation of the apparatus, the drum
A further object is to obtain a resinous product
II is partially ?lled with rosin indicated at 22
of a relatively low melting point which is thermo
and heated to a temperature of approximately
setting and thus may be readily lique?ed and will
450° F. at which point the rosin in the drum
form a solid product upon the further applica
has lique?ed. Suitable ligno-ceilulosic material
tion of heat.
35 such as wood ?bers or particles of relatively low
Other features and advantages of the inven
density are introduced into the hopper I‘! from
tion will appear from the following speci?cation
which they are advanced by the screw conveyor
and drawing, in which
Hi to the inlet M in the drum I l and pass into
Figure 1 is a diagrammatic showing of ap
the drum. The ligno-cellulosic particles form a
paratus for carrying out the reaction and Fig. 40 plug 23 between the inlet Id of the drum H
2 is a sectional view taken along the line 2--2
and the end of the screw conveyor [8. The
of Fig. 1.
plug of ligno-cellulosic particles in the inlet M
In the speci?c embodiment of the invention
of the drum l i serves to seal the inlet to prevent
described herein and referring particularly to
escape of rosin vapor from the drum II through
the drawing, a furnace or heater ll! of any suit
the same. As the screw conveyor I8 is rotated,
able construction is arranged with a container
the plug of wood particles as a whole is advanced,
or drum H of any suitable size and shape sup
the particles at the discharge end being intro
ported therein and adapted to be heated by the
duced into the drum I I.
furnace. The furnace is preferably equipped
As the ligno-cellulosic material is fed into the
with a suitable temperature control ( not shown) 50 drum, the temperature of the rosin is gradually
which permits careful and accurate adjustment
raised and substantially all of the ligno-cellulosic
of the temperature within the furnace. A ?ue
material is added by the time that the temper
l2 extending from the furnace receives the ex
ature of the rosin reaches 550" F‘. The raising
haust gas therefrom. If desired, the drum or
of the temperature of the rosin continues until
container ll may be equipped with a jacket (not 55 the mixture of rosin and ligno-cellulosic material
2,418,826
3
in the drum reaches the neighborhood of 600° F.
The scraper 20 is continuously operated dur
ing the reaction and serves to intimately mix
the particles of the ligno-cellulosic material with
the rosin and continuously agitate the mixture.
The reaction is continued for a substantial period
of time in order to permit all of the ligno-cellu
losic material to react with the rosin.
The re
action is an endothermic one and requires the
addition of a considerable amount of heat to 10
carry it on properly._'After the materials are
mixed the reaction begins and takes up a large
quantity of heat. When the reaction mixture no
longer takes up substantial quantities of heat
the reaction may be considered as being complete
or nearly complete. Ordinarily, the reaction will
require a period of at least one-half hour and
often as long as two or three hours.
When the
reaction is substantially complete the entire mass
in the drum I I is in the liquid state, after which
said mass may be removed from the drum ll
cause local condensation of the rosin vapor on
the same. It may be that the condensation of
the rosin vapor on the wood ?bers to form liquid
rosin facilitates the introduction of ?bers into
the liquid rosin and the mixing of the same there
with by increasing the density of the wood ?bers
and by wetting the ?bers with the condensed
liquid rosin to improve the blending of the ?bers
with the liquid rosin.‘
V
The wood particles or ligno-cellulose may be
added continuously to the heated rosin by means
of the screw conveyor until the proper propor
tions of the reaction ingredients have been ob
tained. At this point the temperature is prefer
ably raised as rapidly as-possible to a tempera
ture in the range of 600° F.-650° F., preferably
between 625° F.—635° F. and the mixture main
tained at this temperature and continuously
agitated until the reaction is substantially com
plete.
Ordinarily, between one-half and two _
hours will be required for the reaction, the time
through the outlet 24 controlled by the valve 25.
By means of the invention it is possible to
utilize ligno-cellulosic products such as wood
varying substantially with the quantities of in
gredients used and with the other conditions of
the reaction. The reaction is preferably carried
?bers which may be in the nature of residues
from other operations or processes. For ex~
out at atmospheric pressure.
ample, the ?nely divided particles of wood ?bers
which are obtained from the acid hydrolysis
a
The exact mechanism of the reaction is not
completely known. Since the reaction occurs at
a temperature to which both the rosin and the
wood particles normally partially decompose, it
of wood and the wood ?bers which have been
may
be that the reaction occurs between the
processed either in steam or organic solvents to 30
decomposition products or partial decomposition
remove therefrom the soluble organic -constitu
products of the rosin and ligno-cellulose. At any
ents thereof are particularly suitable for the
rate, when the reaction is carried out under the
process. Unprocessed ?ber or sawdust is not as
conditions set forth, the materials readily react
desirable as these materials but may in some in
to form a resinous plastic thermo-setting prod
stances be used in the process. It has been
not.
found that the reaction m'ay be carried out, for
In carrying out the reaction, the temperature
example, with pine shavings and alpha-cellulose.
of the mixture in the reaction chamber should
The ligno-cellulosic material should preferably
be very carefully controlled. The rosin should
be in the form of ?nely divided particles. How
be
heated before the ligno-cellulosic material is
~10
ever, if the reaction conditions are very care
introduced. The temperature at which the rosin
fully controlled, it is possible to carry out the
is initially heated prior to the introduction of
reaction using particles of a substantial size.
the ligno-cellulosic ‘material should be in the
By using the screw conveyor [5 to introduce
neighborhood of 450° F. After the material has
the ligno-cellulosic material into the reaction
chamber, the mixing operation may be carefully - been introduced into the rosin the temperature
of the mixture should be raised to approximately
controlled. The material should be introduced.
600° F. and maintained in the neighborhood of
slowly in order to permit the ligno-cellulosic
this temperature until the reaction is substan
material to become mixed with the rosin shortly
tially complete. Preferably, the mixture should
after it is introduced into the container. It is,
be maintained at a temperature of between 625°
50
of course, desirable to introduce the material as
F. and 635° F. as the reaction proceeds.
vrapidly as possible without forming a doughy
In carrying out the reaction various proportions
mass in the rosin. If the material is introduced
of the ingredients may be used. Preferably in
too rapidly, this doughy mass will be formed and
the neighborhood of equal parts of the ligno
will prevent the proper mixing and reacting of
cellulosic material and the rosin are used in the
the ingredients. Nevertheless, in accordance
reaction, the proportions being by weight. Since
with the present invention the ligno-cellulosic
the ligno-cellulosic material, when formed of light
, material may be introduced in a very short time,
wood ?bres, may be of a density as low as 1/20 or
it being possible to completely mix a large batch
Han of that of the rosin, the process in this in
in a few minutes under ordinary conditions.
stance serves to facilitate the incorporation of
By following the reaction conditions set forth,
the ?bres in the rosin.
it is possible to readily incorporate the ligno
The proportions in which the ingredients are
cellulosic material in the liquid rosin without
mixed will, to a certain extent, determine the type
the formation of a doughy mass in the rosin and
of product which is obtained in the reaction.
without any substantial scorching or partial car
65 For example, a reaction between ?fty percent
bonization in the mixture.
‘
ligno-cellulosic material and ?fty percent rosin
Since rosin at a temperature of 450° F. or above
results in a product which has a melting point
possesses a substantial vapor pressure, the
of 260° F. On the other hand, when forty-three
chamber during the course of the reaction con
percent ligno-cellulosic material is reacted with
tains rosin vapor above the liquid rosin. When
?fty-seven percent rosin, the product has a melt
the wood ?bers are introduced into the cham
ing point of approximately 230° ,F., while the
ber, they are brought into contact with this
product of a reaction of forty-?ve percent rosin
vapor before being introduced into the liquid
rosin. The rosin vapor being maintained at an
and ?fty-?ve percent ligno-cellulosic material
elevated temperature serves to preheat the wood
?bers while, at the same time, the cooler ?bers
melts at approximately 295° F. In each instance
the proportions are by weight and the reaction is
anaaac
5 .
6
,
carried on until no Iurthendistillate is obtained
be used as a coating resin particularly when
from the reaction mixture v'at a temperature at
treated with drying oils and the like. As a coat
a range of 625° F. and 630° F.
ing resin the product is particularly useful in pipe
Each of the various products which is obtained
and conduit coverings and the like.
in the reaction is subject to a lowering of the Li
The foregoing speci?c description has been
melting point if the product is reheated at a
given for the purpose of illustrating the inven
higher temperature in the absence of air. For
tion and the means of practicing it. Changes
example, the product obtained by reacting parts
and modi?cations, therefore, may be made in the
of the rosin and ligno-cellulosic material, which
process and product as set forth, particularly as
melts at 260° F., may be reheated at 640° F. to
to the quantities of the reagents used and as to
650° F. in the absence of air to obtain a product
the conditions of the reactions without departing
which melts at approximately 230° F. In each
from the spirit and scope of the invention.
case the heating at a higher temperature in the
We claim:
absence of air will result in the lowering of the
1. A process of forming a resinous plastic ma
melting point. The operation need not be a re 15 terial comprising heating a body of rosin to a
heating operation since the same effect may be
temperature in the range of 450° F.—550° F., in
obtained by heating the product or the original
troducing into the heated body a solid ligno
reaction mixture to 640° F. to 645° F. in the ab
cellulosic material, agitating the mixture, and
sence of air. The product of the reaction between
then heating the same to a reaction temperature
forty-?ve percent and ?fty-?ve percent ligno- ~ until the entire mass has lique?ed, said reaction
cellulosic material, which normally melts at 295°
temperature being at least approximately 600°
F., may be changed to a 230° F. melting point
and not substantially above 650°.
product by heating the material in the absence
2. A process of forming a resinous plastic ma
of air at a temperature in the range of 650° F.
terial comprising, heating a body of rosin to a
to 660° F.
temperature in the range of 450° F.-550° F., in
The products resulting from the reaction are
troducing small particles of wood ?bre into the
in the form of black plastic resins which are
body of rosin, agitating the mixture, raising the
liquid at the reaction temperature. If the prod
temperature of the mixture to 600° F.-650° F.,
uct is withdrawn from the reaction chamber while
and maintaining the mixture at the raised tem
in the liquid condition, it will be found to have 30 perature until the entire mass has lique?ed.
the melting point above stated when tested by the
3. A process of forming a resinous plastic ma
ball and ring method.
"
terial comprising, heating a body of rosin at
When the products of the reaction are heated
atmospheric pressure to a temperature in the
in the presence of air to a temperature above
neighborhood of 450° F., introducing into the body
630° F., preferably in the neighborhood of 650° F.
small ?brous particles of a‘ligno-cellulosic mate
to 660° F., they will gradually solidify to form
insoluble infusible masses. The products, there
fore, are possessed of thermo-setting properties
and are extremely valuable as molding com
pounds.
The thermo-setting resin which is normally
‘ obtained from the reaction in the liquid phase,
may have a melting point of approximately 230°
F. and is, therefore, normally solid. The solid
resin possesses a black opaque lustrous appear
' ance and is quite brittle.
When fractured the
exposed‘ portions of the rosin are brilliant and
rial, the particles being of relatively low density,
intimately mixing the ligno-cellulosic material
with the liquid rosin, increasing the temperature
of the mixture to ,a temperature in the range of
625° F.-635° F., and maintaining the mixture at
a temperature in’Hsaid range while continuously
agitating the same until the entire mass has
lique?ed.
’
4. A process of forming a resinous plastic ma
' terial comprising, heating a body of rosin to a
temperature in: the range of 450° F.-550° F., in
troducing small particles of ?brous ligno-cellu
lustrous.
losic material of relatively low density into the
The reaction product is substantially insoluble
heated rosin, said particles being present in the
in practically all organic solvents with the ex 50 proportion of approximately one part by weight
ception of aromatic naphthas and carbon tetra
to each part by weight of rosin, agitating the
chloride. Such solvents as para?inic naphthas,
mixture, raising the temperature of the mixture
gasolines, greases, oils, etc., do not affect the
to 600° F.-650° F., and maintaining the mixture
material. In addition, the resinous material is
at the raised temperature while continuously agi
resistant to organic and mineral acids and to 55 tating the same for a period of at least one-half
caustic solutions in concentrations up to ten per
hour to "permit the ligno-cellulosic material to
cent.
react substantially completely with the rosin.
The reaction product may be used in further
5. A process of forming a resinous plastic ma
. reactions to obtain desired materials.
It may,
terial comprising providing a substantially closed
for example, be reacted with drying oils .such as 60 container having therein a quantity of heated
tung oil or linseed oil to form a new type of
rosin, the rosin being in the liquid state and at
coating plastic resin as distinguished from mold
a temperature of approximately 450° F., grad
ing plastics. For this type of reaction, a mixture
ually raising the temperature of the rosin to 550°
of twenty-?ve percent to thirty percent of the oil
F. while slowly introducing into the same small
with seventy to seventy-?ve percent of the res 05 ?brous wood particles of relatively low density,
inous material is preferably used. The product
of such a reaction is soluble in mineral spirits
and will produce tough ?lms of high luster and
jet black re?ection. Such products are extreme
intimately mixing the wood particles with the
liquid rosin, raising the temperature of the mix
ture to a temperature in excess of 600° F., and
below the decomposition temperature‘ of the res
ly useful in the preparation of coating ?nishes. T0 inous reaction products and maintaining the mix
The rer'.:ous plastic product of the reaction
ture at a temperature in excess of 600° F. while
between .116 rosin and ligno-cellulosic material
agitating the same for a substantial period of
...ay be used as a molding resin and is particu
' time to permit the entire mass to liquefy.
larly valuable because of its thermo-setting prop
6. A process of forming a resinous plastic ma
erties. On the other hand, the product may also 75 terial comprising, providing a body of heated
8,418,826
7
.
rosin at a temperature in the range of 450° F.
ture being maintained at the raised temperature
550° F., introducing into the body small particles
01' ligno-cellulosic material, intimately mixing the
ligno-cellulosic material with the rosin, raising
the temperature of the mixture to 600° F.-650°
F., and maintaining the mixture at the raised
in the presence of air.
substantially the melting point of pure rosin,
mixing the resulting molten material with the
ligno-cellulosic material .in approximately equal
temperature for a period of at least several hours
while simultaneously agitating the mixture.
7. A process of forming a resinous plastic ma
substantially above 650‘ E, and maintaining the
,
8. A process which comprises heating rosin to
proportions by weight, then heating the mixture
to a reaction temperature above 800° F. and not
terial comprising, providing a body of heated 10 mixture at that temperature for a period oi at
least approximately one-half hour.
liquid rosin, introducing into said body small par
9. The method as set forth in claim 8, in which
ticles of a ligno-cellulosic material, raising the
the reaction is carried out at a temperature oi
temperature of the mixture to a temperature in
GOO-635° F., and the reaction product is then
excess of 650° F., and below the decomposition
temperature or the resinous reaction products, 15 heated in the absence of air at a temperature
above 640° F.
maintaining the mixture at the raised tempera
ture for a substantial period of time until the
reaction between the ligno-cellulosic material
and the rosin is substantially complete, the mix-
FREDERICK W. KRESSMAN.
FREDERICK W. KRESSMAN, JR.
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