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Патент USA US2114392

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Patented Apr. 19, 1938
,
UNITED STATES
PATENT
2,114,392
OFFICE
'
2,114,392
PLASTICIZED PINE WOOD PITCH AND
METHOD OF PRODUCING
Fred H. Lane, Hillsdale, N. Y., assignor to Her
cules Powder Company, Wilmington, DeL, a
corporation of Delaware
No Drawing. Application May 31, 1935,
Serial No. 24,356
9 Claims.
(Cl. 134-26)
_
different methods of puri?cation of rosin.
A
This invention relates to a plasticized pine
wood pitch and to methods for producing the
comparison of the properties of three pine wood '
same.
pitches is given in the following table, in which
Extracted pine wood pitch, which is complex
5 resinous material whose exact composition is un
known, comprises the residue left after the sep
aration of rosin, turpentine and other more val
uable constituents of pine wood. It has been
found to be a valuable resin for use in insula~
10 tion, varnishes, and the like. However, a rather
marked brittleness possessed by the extracted
pine wood pitch has rendered it less valuable for
many purposes than would otherwise be the case.
Extracted pine wood pitch, as has been indii
' cated, is obtained in connection with the produc
tion of wood rosin from; pine wood. The pine
wood pitch will comprise a residue low in abietic
acid remaining after the separation of re?ned
rosin high in abietic acid from the resinous mate
a
—0 rial obtained by extraction of pine wood with a
solvent. It is characterized by substantial insol
ubility in cold petroleum hydrocarbons, but will
differ somewhat in its speci?c characteristics,
such as acid number, melting point, exact petro
25 leum ether solubility and content of naphtha
and toluol soluble matter, depending upon the
method for the recovery of rosin from pine wood
used in its production.
'
'
Pitch A is that obtained by extraction of wood
with hot petroleum solvents subsequent to the
removal of the volatile oils by steam distillation,
re?ning with furfural, evaporation of the furfur
al and a ?nal extraction of the residue with
petroleum solvent to remove petroleum soluble
matter. Pitch B is that obtained by a benzol ex 10
traction of unsteamed wood, evaporation of the
benzolsolution to a residue, extraction of the
residue in hot low boiling petroleum solvent, pre
cipitation of the Pitch B by washing with cold
water, and then removal of this precipitate by
?ltration. Pitch C is obtained by the evaporation
of the furfuralflayer, after re?ning of the gaso
line solution of the crude resin obtained by the
benzol extraction of pine wood.
V20
Pitch A Pitch B Pitch C
Melting point (Hercules drop method).
Acid number ________________________ __
Unsaponi?able matter _ _ _ _ _ _ . . _ _ _
V. M. & P. naphtha insolubleToluol
91° 0
100
_ . _ . _ . _ __
_
soluble . . _ _ _ . _ _ _ _ . .
115° C.
102° 0.
105
116
5%
8
a
89. 5%
96%
83 o
_ _ _ _ _ _ __
40%
98%
Petroleum ether insoluble
92. 0%
Saponi?cation number. . _
______ __
169
140
Ash __________________________________________ __
036%
99%
. 022%
95%
As is well known, rosin is extracted from pine
with live steam to remove volatile oils, such as
It is often desirable to subject the extracted '30
pine wood pitch to a .heat treatment at about
200°-250° C, to reduce a certain tendency to foam
turpentine and pine oil. Again, volatile oils, as
turpentine, and pine oil, are extracted with the
rosin without ?rst steaming for their removal.
Following extraction the extract is distilled for
possessed by the untreated pitch. Such heat
treatment will change the physical properties of
the pine wood pitch to some extent. Thus, Pitch
B when heat treated has the following charac
wood by the use of a suitable solvent, such as hot
gasoline, or benzol after steaming of the wood
the removal of solvent where the wood was sub
jected to steaming before extraction and for the
rem-oval of solvent and volatile oils, as turpentine
and pine oil, where the wood was extracted di
rectly without steaming. As the result of dis
tillation a resinous material containing abietic
acid and admixed impurities is obtained. This‘
resinous material may be treated in any one of
a number of ways, all known to the art, for the
removal of re?ned rosin high in abietic acid. The
residue remaining after the removal of re?ned
rosin and comprising a dark colored, hard, resin
-u' ous mass low in abietic acid constitutes the pine
wood pitch.
The exact properties of the pine wood pitch
obtained as indicated above will depend upon the
teristics:
.
,
,
-
Heat treated Pitch B
Melting point, (drop method) -Degree C.____ 120 40
Acid number__-_ ____________________ _____..
83
Unsaponi?able matter _______ __Percent'___..
10
V. M. & P. naphtha insoluble ____ __do____ _..
9'7
_Toluol soluble __________________ __d0 ____ __
80
Petroleum etherinsoluble _______ __do____._-
99 45
Saponi?cation number_____- _________________ __
Ash _____ __
Percent
..
.040
As has been said, the extracted pine wood pitch
su?Eers to some extent from a brittleness which 50
interferes with its use in certain ways. Now in
accordance with this invention it has been found
that this brittlenessmay be greatly reduced or
method used for. original extraction from the ' eliminated without sacri?cing any of the valua
ble electrical and solubility characteristics of the 55
wood. when the wood is steamed before sol
vent extraction, a pine wood pitch is obtained pine wood pitch by admixing a natural glyceride,
having somewhat different properties from that as an animal or vegetableoil, with the pine wood
‘
obtained when the wood is extracted without pitch.
steaming. Likewise the properties of pine wood
The natural glyceride may be an animal or
60 pitch are somewhat different when obtained by vegetable oil, as, for example, castor oil, polymer
2
2,114,392
'ized castor oil, soya bean oil, cottonseed oil,
China-wood oil, cocoanut oil, Perilla oil, olive oil,
linseed oil, etc., and may be mixed with the ex
tracted pine wood pitch in widely varying
amounts, depending on the degree of ?exibility
or pliability desired and the use for which the
plasticized product is intended. A range of from
about 1% to about 70% oil may be cited as typical
of the variation in oil content that may be used.
10 While any natural glyceride may be used, the use
of castor oil, either raw, blown, or polymerized,
is preferred where the product is to be used in
electrical insulation or will be exposed for long
periods to the action of petroleum hydrocarbons.
15
The extracted vpine wood pitch and the natural
glyceride may be mixed and ‘combined by dis
solving them together in desired proportions in
a volatile solvent, as, for example, ethyl alcohol,
ester solvents, cyclic hydrocarbons, etc., with the
20 use of heat if desired, and then evaporating the
solvent. However, a preferred procedure is‘ to
combine and blend the oil and pine wood pitch
by fusing the pine wood pitch at a temperature
slightly above its melting point and then adding
25 and thoroughly mixing with the fused pitch the
desired amount of animal or vegetable oil. The
mixture is then allowed to cool and is ready for _
use.
.
The following table shows the physical proper
ties of various-plasticized pine wood pitch prod
ucts in accordance with this invention:
TABLE
36
Ordinary castor oil
with heat-treated
Pale blown castor oil
with heat-treated
pitch A
40
Castor oil ________ _.
Gasoline insoluble.-
pitch A
5%
94. 7
8%
94. 5
15%
92. 5
107
109
105
106
109
97
V. B. " V. B.
‘B.
V. B.
V. B.
B.
Melting point .... __
5%
93. 8
8%
87. 4
15%
84. 7
products marked “B.” may well have sufficient
pliability in’ a ?lm form to be used in varnishes,
etc.
'
Other pine wood pitches give substantially simi
lar results when admixed with castor oil as those
shown ‘above for Pitch A. The results obtained
by using other animal or vegetable oils in place
of castor oil will also be similar, except the gaso
line insolubility may not be so high.
It will be understood that the details and ex 10
amples hereinbefore set forth are illustrative only,
and are in no way in limitation of the invention
as ‘herein broadly described and claimed.
What I claim and desire to protect by Letters
Patent is:
~
1. A plasticized product characterized by low
solubility in petroleum hydrocarbons comprising
15
a mixture of a natural glyceride and a petroleum
hydrocarbon-insoluble resin obtained by ?rst, ex
tracting pine wood with a coal tar solvent, sec 20
and, removing the volatile constituents from said
extract and leaving a residual resin, then third,
extracting from said residual resin and by means
of a petroleum hydrocarbon solvent, the petrole
um-soluble non-volatile constituents of said re 26
sidual resin.
2. A plasticized product characterized by low
solubility in petroleum hydrocarbons comprising
a mixture of a vegetable oil= and a petroleum hy
drocarbon-insoluble resin obtained by ?rst, ex~ 30
tracting pine wood with a coal tar solvent, second,
removing the volatile constituents from said ex
tract and leaving a residual resin, then third, ex
tracting from said residual resin and by means
of a petroleum hydrocarbon solvent, the petrole 36
um-soluble non-volatile constituents of said re- ~
sidual resin‘.
3. A plasticized product characterized by low
solubility in petroleum hydrocarbons comprising
a mixture of a castor oil and a petroleum hydro
carbon-insoluble resin obtained‘ by ?rst, extract
ing pine wood with a coal tar solvent, second, re
moving the volatile constituents from said extract _
Polymerized castor oil fused together
45
and leaving a residual resin, then third, extract
ing from said residual resin and by means of a 45
Pitch A
petroleum hydrocarbon solvent, the petroleum
Castor oil ........ __
Gasoline insoluble._
5%
97.3
Melting point .... _.
8%
97.6
15%
94. 9
25%
96. 5
107
105
98
87
V. B.
V. B.
B.
P
33%
96. l
50%
90. 7
85
74
V. P.
S
50
soluble non-volatile constituents of said residual
resin.
_
4. A plasticized product characterized by low
solubility in petroleum hydrocarbons. consisting 60
.of between about 1% and 70% of a natural glycer
Heat-treated pitch A
ide in a mixture of a natural glyceride and a pe
troleum hydrocarbon-insoluble resin obtained by
55
Castor oil ________ __
5%
8%
15%
33%
.50%
Gasolineinsolubla.
96.7
96.4
95.9
93
93
93
Melting point ____ ._
112
111
ill
93
90
83
B
P.
V. P.
S.
> ‘
'
V B
V. B.
_ ?5%
_
_
Polymcrized castor oil blended in a solvent
60
Heat-treated
pitch A
_
PltCh'A
?rst, extracting pine wood with a coal tar solvent,
second, removing the volatile constituents from
said extract and leaving a residual resin, then
third, extracting from said residual resin and by
means of a petroleum hydrocarbon solvent, .the
petroleum-soluble non-volatile constituents of
60
‘said residual resin.
5. A plasticized product characterized by low
solubility in petroleum hydrocarbons consisting
Castor oil ____________________________ __
65
Gmolme insoluble
_. __-
Melting point ________________________ __
5%
15%
25%
93
89
94
119
1m
93
V. B.
B.
B.
Notes:
S.—Denotes extremely soit, rubbery and sticky.
B.—Denotes brittle.
70
_
V. B.—Denotes very brittle.
'
.
-
P.—Denotes pliable and capable of being moulded with
lingers.
.
V. P.—-Denotes very pliable.
It is to be noted, however, that the ratings 8.,
B., V. 13., etc. are only comparative and repre
75 sent the brittleness in the mass. Accordingly
of between about 1% and 70% of a vegetable. oil
in a mixture of a vegetable oil and a petroleum
hydrocarbon-insoluble resin obtained by ?rst,
extracting pine wood with a coal tar solvent,
second, removing the volatile constituents from
said extract and leaving a residual resin, then
third, extracting from- said residual resin and by
means of a petroleum hydrocarbon solvent, the
petroleum-soluble non-volatile constituents of
said residual resin.
.
I
6. A. plasticized product characterized by low
solubility in petroleum hydrocarbons consisting of
between about 1% and 70% of castor oil in a
65
2,114,992
mixture of castor oil and a petroleum hydrocar
bon-insoluble resin obtained by ?rst, extracting
pine wood with a coal tar solvent, second, re
. moving the volatile constituents from said extract
5 and leaving a residual resin, then third, extract
ing from said residual'resin and by means of a
petroleum hydrocarbon solvent, the petroleum
soluble non-volatile constituents of said residual
resin.
'
1o
‘7. The method of producing a plasticized prod
uct characterized by low solubility in petroleum
hydrocarbons which comprises mixing a natural
glyceride, in amounts between about 1% and ‘70%
of the mixture, with a petroleum hydrocarbon
15 insoluble resin obtained by ?rst, extracting pine
wood with a coal tar solvent, second, removing
3
insoluble resin obtained by ?rst, extracting pine
wood with a coal tar solvent, second, removing
the volatile constituents from said extract and
leaving a residual resin, then third, extracting
from said residual resin and‘ by means of a pe
troleum hydrocarbon solvent, the petroleum-sol
uble non-volatile constituents of said residual
resin, the admixture being effected by fusing the
said resin, mixing the glyceride with thefused‘
resin and thereafter cooling the'mixture,
9. The method of producing a plasticized prod
10
uct characterized by low solubility in petroleum
hydrocarbons which comprises mixing a natural
glyceride, in amounts between about 1% and 70%
of the mixture, withv a petroleum hydrocarbon 15
lnsoluble resin obtained by ?rst, extracting, pine
the volatile constituents from said extract and » wood with a‘ coal tar solvent, second, removing
leaving a residual resin, then third. extracting
from said residual resin and by means of a pe
the volatile constituents from said extract and
leaving a residual resin, then third, extracting
20 troleum hydrocarbon solvent, the petroleum-sol
from said residual resin andv by means of a 20
uble non-volatile constituents oi said residual. petroleum hydrocarbon solvent, the petroleum
resin. .
soluble non-volatile constituents of said residual
8. The method of producing a plasticized prod
resin, the admixture being e?ected by dissolving
uct characterized by low solubility in petroleum
25 hydrocarbons which comprises mixing a natural
glyoeride, in amounts between about 1% and 70%
01' the mixture, with a petroleum hydrocarbon
the said resin and the natural glyceride in a-vol-;
uble solvent and then evaporating the solvent. 25
FRlilDH. LANE.
I
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