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Патент USA US2115490

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Patented Apr. 26, 19.38
2,115,490 .
UNITED STATES PATENT OFFICE
2,115,490
METHOD OF PURIFYING ROSIN
‘Irvin W. Humphrey, Wilmington, Del., assignor
to Hercules Powder Company, Wilmington,
Del., a corporation of Delaware
'
No Drawing. Application July 27, 1936,"
Serial No. 92,846
9 Claims.
This invention relates to an improved method
of purifying rosin.
Heretofore, several methods for the removal of
(01. s7-2) .
in order to facilitate contact of the rosin with
the silico?uoride.
-
I may carry out the silico?uoride treatment of
the rosin in a solvent at room temperatureor at
an elevated temperature, and I may employ vig- 5
visible and latent color bodies from‘ rosin have
5 (been known, among them the treatment of a
gasoline solution of rosin with furfural, aniline, . o-rous agitation during the treatment to promote
phenol, liquid sulfur dioxide, etc, separation of thoroughness of contact of the silico?uoride with
the selective solvent containing the color bodies the rosin and thus shorten the time of treat
ment necessary to attain the re?ning action de
and low-grade rosin, and recovery from the gaso
10 line solution of the puri?ed rosin. However, cer-. sirable. In case of the use of a suspension of a W .
slightly-soluble silico?uoride, I may, after treat
tain of the darker grades of rosin have not re
sponded to such treatment to as great an extent ment of the rosin therewith, filter the solution
as is desirable, so that, while an improvement in and suspension to remove the suspended silico
color grade by such treatment results, such treat— ?uoride, and then wash the rosin solution with
.
15
'15 ment will not bring certain of the very dark rosins water. ‘
After my re?ning treatment with silico?uoride,
up to the very light color grades.
The method in accordance with my improved the rosin solution is subjected to a second refin
process enables me to re?ne very dark color ' ing treatment with any of the usual color body
selective reagents, e. g., furfural, phenol, resor
grades of rosin to the very palest color grades.
The method in accordance with my invention cinol, or other selective, immiscible color body 20
consists broadly in the treating of a solution of solvent or mixtures thereofwhich do not interact
rosin in a water-immiscible solvent therefor with one with another, or by fuller’s earth, activated
a silicofiuoride (including hydrogen silico?uoride, carbon, etc. The rosin recovered from the rosin‘.
2
or hydro?uosilicic acid), followed by a selective
color body removal treatment of the rosin-solvent
solution. Such combined re?ning treatment of
rosin accomplishes a re?ning action not attain
able by either re?ning treatment alone.
While the greatest advantage of my improved
solvent after silico?uoride or combined refining!
treatment may be further puri?ed by crystalliza- 25
tion, heat treatment, distillation under reduced
pressure, fractionation, partial hydrogenation, or
any combination thereof, since the real effect of
the silico?uoride treatment in ‘my process is to
30 process of re?ning rosin lies in the treatment of
the darker color grades of rosin, either wood or
place the dark rosin in such a state that it is 30
gum, I may use the same to advantage upon any
color grade of rosin to be refined.
In practicing the method in accordance With
35 my invention, the rosin solvent used may be a
hater-immiscible solvent for the rosin, for ex
ample, mineral spirits, gasoline, butane, petro
leum ether, pentane, hexane, etc. ‘The silico?u
oride employed in my re?ning treatment may be
4.0 a water-soluble silico?uoride, e. g., silico?uorides
'
of sodium or potassium‘ or ammonium, aniline
fluosilicate, toluidine fluosilicate, or other organic
?uosilicates, a sparingly water-soluble silico?uo
ride, e. g., calcium or magnesium silico?uoride,
45 titanium-potassium silico?uoride, or ‘a slightly
soluble silico?uoride, e. g., lead silico?uoride. In
the case of the use of silico?uorides of‘ little solu
bility in water, I prefer to use the same as a sus
pension in water, so that during the treatment
50 in accordance with my invention the water is
continuously saturated with the silico?uoride em
ployed. Also, in the case of use of silico?uorides
slightly soluble in water, but soluble in dilute a1
cohol, I may use a dilute alcohol solution thereof
55 in the treatment of the rosin solvent solution,
readily re?nable by the subsequent selective re
agent or other treatment, whereas without suchv
preliminary treatment, it is resistant thereto.
As an example of the process in accordance
with my invention, a 20% gasoline solution of 35
gum D rosin was washed thoroughly by agita
tion with one-half its volume of a 1% aqueous
solution of sodium silico?uoride, the sodium sili
co?uoride being partly in solution and partly in
suspension, the two layers of liquid allowed to 40
separate, the gasoline solution of rosin decanted.
This gasoline solution of rosin was then given
three successive washes, each amounting to one
?fth of the rosin‘ solution, with furfural at 0° C.,
the furfural solution allowed to settle, the gaso- 45
line solution of the puri?ed rosin decanted, the
gasoline evaporated, and the rosin. recovered.
The recovered rosin graded M in color, and on
' heat- bleaching formed a rosin grading X in color.
As‘ an additional example of the process in 50
accordance with my invention, a 50% solution of
gum D rosin in gasoline, containing 65 g. of rosin,
was given two washes with an aqueous solution
of sodium silico?uoride containing 0.3 g. of sodi
umsilicofiuoride per wash, then the rosin was sub- 55
2
2,1 15,490
jected to the usual furfural re?ning treatment.
The rosin recovered was WG‘ in color, and heat
bleached to better than X grade on heating to
about 300° C. for 10 minutes. When the sodium
silico?uoride treatment was omitted, the furfural
re?ned rosin was G in color and heat-bleached
only to a WW grade. Similarly, a gum D rosin,
which re?ned to an N grade with furfural alone,
was re?ned to an X grade when the preliminary
10 silico?uoride treatment was given, and gum E
rosin, re?nable to M grade by furfural only, re
?ned to a WG grade by inclusion of the silico
?uoride treatment.
To illustrate the cooperation of the two treat
ments and the unexpected advantages resulting
from such combination of treatments, another
portion of the gasoline solution of gum D rosin
used inthe above treatment was subjected to
‘the silico?uoride wash alone, and the rosin re
20 covered from the gasoline layer. The recovered
rosin graded D in color, and no appreciable re
?ning action had occurred.
Rosin, subjected to the silico?uoride treatment
alone, when recovered from the solvent is gen
erally found to have undergone no appreciable re
?ning in color grade, but is found to be more
amenable to the action of subsequent re?ning.
I do not limit myself to any particular appa
solution of sodium silico?uoride, separating said
silico?uoride solution from the rosin solution.
thus rendering the rosin readily re?nable by sub
sequent treatment, treating the rosin solution
with furfural, removing furfural and color bodies
from the rosin solution for recovery of puri?ed
rosin.
‘
4. Method of purifying rosin in solution in a
water-immiscible solvent therefor which includes
treating said rosin solution with an aqueous me 10
dium containing a silico?uoride which is at least
appreciably soluble in said aqueous medium, sep
arating the rosin solution from the said aqueous
medium, thus rendering the rosin readily re
?nable by subsequent treatment, treating the ros
15
insolution with a selective color body removing
agent, and recovering puri?ed rosin.
5. Method of purifying rosin in solution in a
water-immiscible solvent therefor which includes
treating said rosin solution with an aqueous so
lution of a silico?uoride, separating said silico
?uoride from the rosin solution thus rendering
the rosin readily re?nable by subsequent treat
ment, treating the rosin solution with a selective
color body removing agent, and recovering puri
25
ratus for the carrying out of my process, nor to
the use of any particular temperature in such
treatment, nor to the use of any particular con
centrations of the reactants, it being obvious
?ed rosin.
6. Method of purifying rosin in solution in a
water-immiscible solvent therefor which includes
treating said rosin solution with a suspension so
lution of a water-soluble silico?uoride, separating 30
the rosin solution from the said suspension solu
tion of silico?uoride, thus rendering the rosin
that different grades of rosin will require various .
readily re?nable by subsequent treatment, treat
modi?cations of the same. I may also apply my
improved re?ning treatment to other resin de~
removing agent, and recovering puri?ed rosin.
rivatives, such as rosin esters, with advantage.
What I claim and desire to protect by Letters
Patent is:
1. Method of purifying rosin which includes
40 treating rosin in solution in a hydrocarbon sol
vent therefor, which hydrocarbon solvent is sub
stantially immiscible with a color body selective
solvent, with an aqueous solution of silico?uoride,
thus rendering the rosin readily re?nable by sub
ing the rosin solution with a selective color body
7. Method of purifying rosin in solution in a
water-immiscible, aliphatic, hydrocarbon solvent
therefor, which includes treating said rosin so
lution with an aqueous medium containing a sili
co?uoride which is at least appreciably soluble in
said aqueous medium, separating the rosin solu
tion from the said aqueous medium, thus render
ing the rosin readily re?nable by subsequent
sequent‘treatment, removing said silico?uoride
treatment, treating the rosin solution with a
selective color body removing agent and recover
solution from the rosin solution, treating the
ing puri?ed rosin.
rosin solution with a selective color body solvent
8. Method of purifying rosin in solution in a
substantially immiscible with the rosin solvent,
removing said color body solvent and color bodies
from the rosin solution, removing solvent from
water-immiscible, aliphatic, hydrocarbon solvent
the rosin solution for the recovery of puri?ed
rosin.
2. Method of purifying rosin which includes
treating rosin in solution in a hydrocarbon solvent
55 therefor, which hydrocarbon is substantially im
miscible with a color body selective solvent, with
an aqueous solution of a silico?uoride, thus ren
dering the rosin readily re?nable by subsequent
treatment, removing said silicofluoride solution
40 from the rosin solution, treating the rosin solu
tion with furfural, removing furfural and color
bodies from the rosin solution, removing solvent
from the rosin solution for recovery of puri?ed
rosin.
3. Method of purifying rosin which includes
treating rosin in gasoline solution with an aqueous
therefor, which includes treating said rosin so
lution with an aqueous solution of a silico?uoride,
separating said silico?uoridc solution from the
rosin solution thus rendering the rosin readily
re?nable by subsequent treatment, treating the
rosin solution with a selective color body remov
ing agent and recovering puri?ed rosin.
9. Method of purifying rosin in solution in a
water-immiscible, aliphatic, hydrocarbon solvent
therefor, which includes treating said rosin solu
tion with a suspension solution of a water-soluble
silico?uoride, separating the rosin solution from 60
the said suspension solution of silico?uoride, thus
rendering the rosin readily re?nable by subse
quent treatment, treating the rosin solution with
a selective color body removing agent and re
covering puri?ed rosin.
IRVIN W. HUMPHREY.
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