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J. B. FEDEZR ETAL
3,140,243
LIGHT
MATERIAL
i
V l
4
%
CRUDE
PH ENOL
DISTILLATION
COL.
DISTILLATION
COL.
H EAVY
MATERIAL
P H E NOL
INVENTORS
JACK B. FEDER
JOSEPH L. RUSSELL
BY
ORNEY
2
(Oldershaw) equipped with a time switch operated mag
netic re?ux splitter and further equipped with a column
entry point onto Plate No. 7 up from the pot which side
entry point is equipped with a stop-cock and a glass
U-tube acting as a liquid seal.
The distillation pot is charged with crude phenol, ob
3,140,243
tar.
3,140,243
Patented July 7, 1964
phenol.
process. The art is confronted by the problems of pro 25 tilled overhead and no cyclohexanone in either the early
or later portions of the distillate. The distillate or ?rst
fraction is not pure phenol. The residue or second frac
tion contains the higher boiling materials and may con
by the dehydrogenation of cyclohexanone, cyclohexanol,
tain some phenol. This residue may be recycled to the
or mixtures thereof.
The discoveries associated with the invention relating 30 dehydrogenation step if desired, or an oxygenated cyclo
hexane fraction thereof may be separated and only this
to solutions of the above problems and the objects
fraction recycled to the dehydrogenation step.
achieved in accordance with the invention as described
The ?rst fraction is re-fractionated using equipment as
herein include the provision of:
already described at an initial re?ux ratio of 2 to 1 for
The process for preparing a pure phenol from a crude
removal of water and light ends, at head temperatures
phenol containing at least one oxygenated cyclohexane
between 60 C. and 178 C. Then the re?ux ratio is
derivative as an impurity, which process comprises frac
changed to 20 to l and distillation is continued to a
tionating said crude phenol into at least two fractions,
purity;
distilled (inclusive)
Head
Temp.
Freezing
Sample Point
in C
Point
in C.
178
178
179
Plate No. 7_
Receiver.
Plate No
40. 6
40. 3
40. 6
179
Receiver ______ _.
40. 2
process.
Example 2
The procedure of Example 1 is repeated except that
part and percent by weight, respectively, it being under
the impure phenol is derived by dehydrogenation of an
stood that these examples are presented as illustrative only
60 equal mixture of commercial grades of cyclohexanol and
and are not intended to limit the scope of the invention.
cedures are set forth, in which parts and percent mean
cyclohexanone.
Example 1
3,140,243
Head
distilled (inclusive)
Temp.
Freezing
Sample Point
Point
in C.
in C.
15
9.1 __________________________ t.
179
40. 7
14.
182
Receiver ________ __
32. 2
23.
27.
182
183
Plate No. 7.
Receiver_
40. 75
38. 5
32.
36.
183
183
Plate N 0.
Receiver.
_-___dO ..... _.
40. 85
40. 1
42.
184
47.
184
40. 85
52.7
78.5
184
183
Receiver ________ _.
-__>_d0 ___________ _.
40. 4
40. 7
40v 65
40. 8O
20 26, 1960.
adjustments.
If desired, the ?rst fraction may be removed in differ
ent cuts, such as a sub-fraction containing lower boiling
2,265,939
2,486,342
2,679,535
2,728,795
2,762,760
2,824,048
Oct.
May
Dec.
Sept.
Feb.
25,
25,
27,
11,
18,
1949
1954
1955
1956
1958