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2,410,205
Patented Oct. 29, 1946
UNI-TED; STATES. PATENT OFFICE.
LIGNEOUS RESINOUS COMPOSITION AND
METHOD OF PRODUCING.
MillardlR. Dusenbury, Wilmington, Del.,.assignor,
' to Hercules Powder Company, Wilmington,
Del, acorporation of Delaware
No Drawing. ApplicationJ .ulyr31; ‘1942,.
Serial N 0. 453,041" '
25‘ Claims.
(Cl. 260--—124)
2
1.‘
off. leaving. the impregnated chips. The impreg
Thisinvention relates-to a novelresinous com.
nated‘ chips were placed in. an. autoclave and.
position and a methodofpreparation. More par
ticularly, it is concerned with an improved method
of producing a novel resinous composition from
c.overed.w-itli~55_0‘ parts of distilled water._ The
autoclave was sealedand heated at, a temperature
0152.605’ C.—2.70? C..for. 1.hour.., This resulted in- a
ligneous woodand tothe resulting product.
Now,,in~.accordance withthis invention, ithasv
143 .parts yield of. resin,
beenrfound that a novelresin, useful. for. a wide
Example 3.
Variety. of purposes. may. be. produced. by heating
SiXtyesiXparts of oiticica oil were dissolved in
ligneous wood, which-has beensubstantially com
enough acetone to completely cover 154 parts of
spent, pine wood chips from, which the turpen:
pletely coveredv with water, with a material. se
lectediromthegroup consisting of higher fatty
acids, which contain a conjugated system of.
double bonds; and. their esters,vv at. an. elevated
temperature and. under s'uperatrnospheric. pres.
sure until. the cellular structure, ofv the wood
has disappeared. The'resi'n is recovered‘ as a
residue remaining after removal of thewater solu
tion. Thus, in. accordance with the improved,
tinetrosin and oils had been extracted.' The ‘ace
tone' was distilled off leaving the impregnated;
chips. The impregnated chips were placed in
an autoclave and covered'with 550 parts of dis;
tilledj Water; The, autoclave. was sealed, and
' heated at-‘a temperature of 260° C.-2!70° C. for 1'
hour.
This resultedin a 150 parts yieldof resin.
process of this invention, a novel. resin may. be
Example 4-
produced by heating. aligneous wood, water and 20
'
Onehundred parts ofloiticica oil'were-dissolved
a material selected from thegroup consisting of
higher fatty. acids, which contain a conjugated
system ofdoublebondsand their esters, ,at a tem
perature within the range of ‘from about 240° C.
to about 330° 6., under superatmospheric pressure
until the cellular structure, of, the wood has dis
appeared, the water being present in‘ suiiicient
amount to. substantially completely cover the
wood,.then recoveringa resinas' the residue re
maining after removal of the water solution.
30
Now, having indicated; in a_ general way, the
nature andpurpose, of.‘ this invention, the. follow
ing examples are illustrative of the invention and
are not to be construed‘ as limiting the,v same.
v
In
in-enough-acetone to completely cover 100 parts of‘
spent pine wood chips from which the turpentine,
rosin» and‘ oils- had beenv extracted: The acetone
was distilled" off leaving the impregnated‘ chips.
The impregnated chips'were; placed in an‘ auto
clave and covered with 5'50Qparts. of‘v distilled
water. The autoclave was sealed and heated at‘
a" temperature of5260°'C.'-2<70‘°“C. for 1‘l hour. This
resulted in a- 130‘ parts yieldof-resin'.
Example. 5.
One hundred parts of the fatty acids derived‘
from'tung oil were dissolved in enough- alcohol
to completely cover lGOparts oil spent pine wood
the examples the ingredients are given in parts
35 chips from whichrthewturpentine, rosin and oils
by weight unless otherwise indicated.
had'beeni extracted. The alcohol was distilled‘
Example 1v
off- leaving the impregnated- chips. The impreg
natedi chips were- placed in- an- autoclave and
Sixty-six parts ofv the‘fatty acids derived'from
. covered with 500 parts of water. The autoclave
tung oil were dissolved in enough acetone to com
pletely cover 154 parts of spent pine wood chips 40 was sealed' and heated} at‘ a» temperature of" 315°
C.-320° C. for 30‘ minutes. A hard; brittle resin
from which the turpentine, rosin and oils had
been extracted.
was produced.
The acetone was distilled o?
'
Example 6‘
leaving the impregnated chips. Theimpregnated
chips were placed in an autoclave and covered
with 550 parts of distilled Water. The autoclave‘ 45
was sealed and heated at- a temperature of 260°
C.-2'70° C. for 1 hour. This resulted in a 119
parts yield of a hard resin.
Sixty-six: parts of- the fatty acids derivedzfrom
tung‘oilwere diSSOlVEdElIl enough acetone‘to com
pletely cover I54v parts of spent'pinewood'chips;
from which the turpentine, rosin and‘ oils have
been‘ extracted?
The acetone was evaporated,
Example. 2
50 leavingithe'iinpregnatedmhips: The impregnated‘
chips. were placed in‘ an’ autoclave and covered:
One hundred) parts of the fatty acids derived
from tungv oil‘ were. dissolved in enough acetone
' with 600- parts- of; Water.
to completely’ cover 100~parts of‘ spent pine- wood
chipsfrom-Which theturpentineh rosin and oils
had been extracted.
The‘ acetone was distilled. 55
The autoclave was
sealedv andsheatedat, a. temperature of- 245° C.
250° C. for: 2 hours. A, hard,_ brittle resin, wasv
thereby.» produced.
2,410,205
3
4
In the above examples, oiticica oil and the fatty
a drop melting point generally above 50° C. and
acids derived from tung oil have been used as the
higher unsaturated fatty acids which contain a
may be as high as about 200° C.
This novel resin is useful for a wide Variety of
conjugated system of double bonds and their
purposes. It may be used in molding composi
esters, The process may be accomplished by the
tions and plastics, as a dry core binder, in core
use of any other higher unsaturated fatty acid,
oils and core oil emulsions, in asphalt emulsions,
which contains a conjugated system of double
as a binding material for ?ber building board, in
bonds and its ester, such as for example, the
dense pressed boards and in bonding insulation
fatty acids from oiticica oil and the like. The
boards.
mixtures of higher unsaturated fatty acids, which 10
What I claim and desire to protect by Letters
contain a conjugated system of double bonds and
Patent is:
their esters as they occur in vegetable oils, animal
1. The method of producing a resinous compo
fats and waxes, may also be employed.
sition which comprises heating a ligneous wood,
While in the examples pine wood has been em
water, and a material selected from the group
ployed as the ligneous wood, other operable lig
consisting of higher fatty acids, which contain a
conjugated system of double bonds and their
neous woods such as maple, birch, basswood, etc.,
may be used. Also the equivalent of “ligneous
esters, at a temperature within the range of from
Wood” and operable in this process, are other lig- about 240° C. to about 330° C. under superatmos
neous materials such as ligneous cellulosic grasses
pheric pressure until the cellular structure of the
wood has disappeared, the water being present in
and straws which are closely related to wood, such
sufficient amount to substantially completely
as, for example, bagasse ?bre, peat moss, and
the like. The wood is preferably used in the form
cover the wood, then recovering a resin as the
residue remaining after removal of the water
of small chips or as sawdust, to facilitate the
penetration of the water during the treatment.
solution.
2. The method of producing a resinous compo
Non-resinous ligneous woods are particularly
sition which comprises heating a ligneous wood,
adaptable for use in this process, but ligneous
water and a higher fatty acid, which contains a
woods which contain up to about 10% by weight
conjugated system of double bonds, at a tempera
of a resin acid may be used. Pine wood from
ture within the range of from about 240° C. to
which turpentine, rosin and oils have been
about 330° C. under superatmos'pheric pressure
steamed and extracted is particularly desirable. ‘
The percentage of the unsaturated higher fatty
until the cellular structure of the wood has dis
acid containing a conjugated system of double
appeared, the water being present in suf?cient
amount to substantially completely cover the
bonds or ester thereof used with the ligneous
wood, then recovering a resin as the residue re
wood treated in accordance with the process of
the invention should be at least 15% and not more
maining after removal of the Water solution.
3. The method of producing a resinous com
than 80% by weight based on the weight of wood,
position which comprises heating a ligneous
and preferably from about 30% to 75%.
The pressure under which the heating proceeds
wood, Water, and an ester of a higher fatty acid,
will fall within the range of from about 400 lbs.
to about 1900 lbs. per square inch. It is desirable
at higher temperature to vent the apparatus so
as to remove some of the volatile gases formed,
such as carbon dioxide. Because of this evolution
which contains a conjugated system of double
bonds, at a temperature within the range of from
about 240° C. to about 330° C. under superat
mospheric pressure until the cellular structure
of the wood has disappeared, the water being
present in sumcient amount to substantially
of these volatile gases, the pressure at which the
completely cover the Wood, then recovering a
process is carried out is usually higher than the
water vapor pressure at the particular tempera
resin as the residue remaining after removal of
ture.
the Water solution.
_
4. The method of producing a resinous compo
The heating may be carried out at a tempera
sition which comprises heating a ligneous Wood,
ture of from about 240° C. to about 330° C., and
preferably from about 250° C. to about 280° C. 50 water, and the fatty acids derivedfrom tung
oil which contain a conjugated system of double
The heating time required in this process is from
bonds, at a temperature within the range of from
about 2 minutes to about 6 hours. At lower tem
peratures, the reaction is slower than at higher.
about 240° C. to about 330° C. under super
atmospheric pressure until the cellular structure
A shortening of the reaction time is also made
of the Wood has disappeared, the water being
possible by a direct injection of the hot water
present in sufficient amount to substantially
into a wood-containing chamber. The type of
wood used and the temperature of heating are
completely cover the wood, then recovering a
resin as the residue remaining after removal of
factors which contribute to vary the heating
time.
the water solution.
5. The method of producing a resinous compo
At the end of the reaction period, the pressure
sition which comprises heating a ligneous Wood,
is released, and the material is cooled. The re
sulting resin is separated from the aqueous solu
Water, and oiticica oil, at a temperature within
the range of from about 240° C. to about 330° C.
tion. If desired, the gases, water and organic ma.
terial may be expelled from the resin by heating
under superatmospheric pressure until the cel
to about 175° C.-275° C. The aqueous layer will 65 lular structure of the wood has disappeared, the
water being present in sufficient amount to sub
usually contain small amounts of acetone, acetic
stantially completely cover the wood, then re
acid, methanol, etc., resulting from the decom
position of the wood.
covering a resin as the residue remaining after
The resulting resinous composition is charac
removal of the water solution.
6. The method of producing a resinous com
terized by freedom from cellular matter remain 70
position which comprises heating a ligneous
ing from the Wood and by a relatively dark color.
wood, water, and ‘fatty acids derived from
It is largely soluble in acetone, cellosolve, carbi
oiticica oil which contain a conjugated system
tol; partly soluble in benzene, toluene, xylene, al
of double bonds, at a temperature within the
cohol, ethylene dichloride, etc., and substantially
range of from about 240° C. to about 330° C. under
insoluble in gasoline hydrocarbons. It Will 113M?
2,410,205
6
the range of from about 240° C. to about 330°C.
superatmospheric .pressure until the cellular
structure of the wood vhasdisappeared, the water
being present in su?icient amount to substan
tially completely cover the wood, then recovering
under superatmospheric pressure until the cel
lular structure of the wood has disappeared, the
water being present in su?icient amount to sub
a resin as the residue remaining after removal UK stantially completely cover the wood, then re
covering a resin as the residue remaining after
of the water solution.
removal of the water solution.
.7. The method of producinga resinous com
13. The method of producing a resinous compo
position which comprises heating pine wood
sition which comprises heating a ligneous Wood,
from which the turpentine, rosin, and ‘oils have
been extracted, water, and a material selected 10 water, and a material selected from the group
consisting of higher fatty acids, which contain a
conjugated system of double bonds and their
fromrthe group consisting of higherliatty acids,
which .contain a conjugated system of double
bonds and their esters, at a temperature within
the range of from about240° C. to‘about 330°‘ C.
under superatmospheric pressure until the cel
lular structure of the wood has disappeared, the
Water being present insu?icient amount to'sub
stantially completely cover the wood, then re
esters, at a temperature within the range of
from about 250° C. to about 280° C. under super
atmospheric pressure until the cellular struc
ture of the wood has disappeared, the water be
ingpresent in suf?cient-amount to substantially
completely cover the wood, then recovering a
resin as the residue remaining after removal of the
water solution.
‘14. Asa new composition of matter, the resin
produced by heating a ligneous wood, water, and
the ‘fatty acids from tung oil which contain a
covering a resin as the residue remaining after
removal of the watersolution.
'
8. .The method of producing a resinous com
position which comprises heating pine .wood from
which the turpentine, rosin, and oils have been
conjugated systemof double bonds at a tempera
extracted, water, and a higher fatty acid, which
ture within the range of from about 240° C. to
contains a conjugated system of double bonds,
about 330° C. under superatmospheric pressure
at aitemperature within the range of from about
until the cellular structure of the'wood has dis
240° .C. to about 330° C. under superatmospheric
appeared, .the water being present in su?icient
pressure until the cellular structure of the wood
amount 'to substantially completely cover the
has disappeared, the water being present in will
cient amount to substantially completely cover 30 wood, then recovering a resin as the residue re
maining after removal of the water solution.
the wood, then recovering a resin as the residue
15. As a new composition of matter, the resin
remaining after removal of the water solution.
produced by heating a ligneous wood, water, and
9. The method of producing a resinous com
oiticica oil at a temperature within the range
of from about 240° C. to about 330° C. under super
position which comprises heating pine wood
from which the turpentine, rosin and oils have
atmospheric pressure until the cellular structure
of the wood has disappeared, the water'being pres—
been extracted. water and an ester of ahigher
fattyacid, which contains a conjugated system
of double bonds, at a temperature within the
range of from about 240° C. to about 330° C.
under superatmospheric'pressure until the cel
lular structure ofthe wood has disappeared, the
water being present in-su?icient amount to sub
stantially completely cover the wood, then re
covering a resin as‘ the residue remaining after
removal of the water solution.
ent in su?icient amount to substantially com
pletely cover the wood, then recovering a resin
40 as the residue remaining after removal of the
water ' solution.
16. As a new composition or matter, .the resin
produced by heating a ligneous wood, water, and
fatty acids ‘derived from oiticica‘oil which contain
on CA . a'con-jugated system of double bonds at a tem
10. The method of producing a resinous com
position which comprises heating pine wood from
which the turpentine, rosin, and oils have been
extracted, water and the fatty acids derived from
tung oil which contain a conjugated system of
double bonds, at a temperature within the range
of from about 240° C. to about 330° C. under
superatmospheric pressure until the cellular
structure of the wood has disappeared, the water
being present in su?icient amount to substan
tially completely cover the wood, then recovering
a resin as the residue ‘remaining after removal .
of the water solution.
11. The method of producing a resinous com
perature within the 'range of from about 240° C.
to about 330° C. under superatmospheric pressure
until the cellular structure of the wood has dis
appeared, the water being present in su?icient
amount to substantially completely cover the
wood, then recovering a resin as the residue re
maining after removal of the water solution.
1'7. As a new composition of matter, the resin
produced by heating pine wood from which tur
pine, rosin, and oils have been extracted,
water, and a material selected from the group
consisting of higher fatty acids, which contain a
conjugated system of ‘ double bonds and their
esters, at a temperature within the range of from
about 240° C. to about 330° C. under super
position which comprises heating pine wood from 60 atmospheric
pressure until the cellular structure
which the turpentine, rosin, and oils have been ex
of the Wood has disappeared, the water being
tracted, water, and oiticica oil, at a temperature
present in su?icient amount to substantially com
within the range of from about 240° C. to about
330° C. under superatmospherie pressure until
the cellular structure of the wood has disap
peared, the water being present in sui?cient
amount to substantially completely cover the
pletely cover the wood, then recovering a resin
. as the residue remaining after removal of the
position which comprises heating pine wood
water solution.
18. The method of producing a resinous compo
sition which comprises heating a ligneous wood,
water, and a higher fatty acid, which contains a
conjugated system of double ‘bonds, at a_ tem
perature Within the range of from about 240° C.
from which the turpentine, rosin, and oils have
been extracted, water, and fatty acids derived
from oiticica oil which contain a conjugated
400 pounds to about 1900 pounds per square inch
until the cellular structure of the wood has dis
wood, then recovering a resin as the residue re
maining after removal of the water solution.
12. The method of producing a resinous com
to about 330° C. under a pressure of from about
system of double bonds, at-a temperature within 75 appeared, the water being present in su?icient
2,410,205
amount to substantially completely cover the
wood, then recovering a resin as the residue re
maining after removal of the water solution.
19. The method of producing a resinous compo
appeared, the water being present in suf?cient
amount to substantially completely cover the
wood, then recovering a resin as the residue re
maining after removal of the water solution.
sition which comprises heating ligneous cellulosic
23. The method of producing a resinous com
material, water, and a material selected from the
group consisting of higher fatty acids which con
tain a conjugated system of double bonds and
position which comprises heating a ligneous wood,
their esters, at a temperature within the range
acids which contain a conjugated system of double
of from about 240° C. to about 330° C. under
bonds and their esters, at a temperature within
the range of from about 240° C. to about 330° C.
under superatmospheric pressure until the cellu
lar structure of the wood has disappeared, the
water being present in sufficient amount to sub
stantially completely cover the wood, then re
covering a resin as the residue remaining after
removal of the water solution.
superatmospheric pressure until the cellular
structure of said ligneous cellulosic material has
substantially disappeared, then recovering a resin
as the residue remaining after removal of the
water solution.
20. The method of producing a resinous com
position which comprises heating ligneous cellu
losic material, water, and a higher fatty acid
which contains a conjugated system of double
bonds at a temperature within the range of from
about 240° C. to about 330° C. under superatmos
pheric pressure until the cellular structure of
water, and from 30% to 75% of a material se
lected from the group consisting of higher fatty
24. The method of producing a resinous com
position which comprises heating for from about
2 minutes to about 6 hours, ligneous wood, water,
and from 15% to 80% of a material selected from
the group consisting of higher fatty acids which
said ligneous cellulosic material has substantially
contain a conjugated system of double bonds and
their esters, at a temperature within the range of
remaining after the removal of the water 25 from about 240° C. to about 330° C. under super
solution.
atmospheric pressure, the water being present in
21. The method of producing a resinous com
sufficient amount to substantially completely
disappeared, then recovering a resin as the residue
position which comprises heating ligneous cellu
cover the wood, then recovering a resin as the
losic material, water, and an ester of a higher
residue remaining‘ after removal of the water
fatty acid which contains a conjugated system 30 solution.
>
of double bonds at a temperature within the range
25. The method of producing a resinous com
of from about 240° C. to about 330° C. under su
position which comprises heating a ligneous wood,
peratmospheric pressure until the cellular struc
water, and a material selected from the group
ture of said ligneous cellulosic material has sub
consisting of higher fatty acids which contain a
stantially disappeared, then recovering a resin as 35 conjugated system of double bonds and their es
the residue remaining after the removal of the
ters, at a temperature within the range of from
water solution.
about 240° C. to about 330° C. under superatmos
22. The method of producing a resinous com
pheric pressure until the cellular structure of the
position which comprises heating a ligneous
wood has substantially disappeared, the water
wood, water, and from 15% to 80% of a material 40 being present in su?icient amount to substantially
selected from the group consisting of higher fatty
completely cover the wood, then recovering a
acids which contain a conjugated system of double
resin as the residue remaining after removal of
bonds and their esters, at a temperature within
the water solution, and heating said resin to from
the range of from about 240° C. to about 330° C.
175° C. to 270° C. to expel the volatile material.
under superatmospheric pressure until the cellu 45
lar structure of the wood has substantially dis
MILLARD R. DUSENBURY.
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