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Патент USA US2136966

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Nov. 15, 1938.
‘Filed Sept. 25, 1956
Patented Nov. 15, 1938
Alwin C. Cams, La Salle, Ill., assignor to Oarus
Gh?mical Company, Inc., avcorporation oi’ Illi
Application September 25‘, 1936, Serial No. 102,609
3 Claims. (Cl. 202-46)
r.‘E'nis method relates to the manufacture of
quinone and other like substances in which the
product is distilled from a reaction mass with
’ The distillation of quinone and other 'or-.
ganic bodies by steam distillation has long
been practiced, but in the preparation of qui
none and certain other organic materials by
steam there is a tendency for the quinone to con
10 dense and form a cake in the condenser which
eifectively blocks the distillation operation.
ture may be such as is obtained by oxidizing
aniline with manganese compounds. Distillate
passes off through the line It into the condenser
5, the mouth 6 of the line I being within the
body of water 1 in the condenser. The water is
circulated through the line l2 by the pump I3
into the extraction vessel l5, wherein a layer of
solvent is maintained. A cooling coil ['6 may be
supplied therein for cooling the solvent. The
arrangement shown is for a solvent heavier than 10
It has now been discovered that this di?iculty ‘water, but where a lighter ‘solvent is used the
may be overcome providing the concentration of flow may be reversed. The washed water passes
through the line I‘! controlled by the valve l8
the quinone in the water condensate is kept be
and back to the condenser 55.‘
15 low saturation, and preferably well below satura
A vacuum is maintained within the condenserv
- tion to such an
extent that no cake is formed. 5 by
the pump Ill, both for the purpose of facili
This result may be accomplished by condensing
the evaporation of quinone in the still and
the steam in an excess of water which is con
also to cool the water within the condenser by
20 moval of the quinone from this water'.. From the boiling. The boiled water is condensed within
- standpoint of economy, however, it is preferred the re?ux condenser IS. A line 20, controlled by 20
to recirculate the water, and this is particularly ' valve 2|, may lead from the solvent vessel I4 to
the condenser tubes and may be employed to
true because it is impossible to completely re
move the quinone therefrom. Preferably, this wash out the condenser of quinone, if necessary,
by circulating some of the washed water there
25 result is accomplished by removing the water
The valves IB and 2| may be kept
before it has become concentrated or saturated
with quinone and removing the quinone, or some partially open, if desired, to maintain a higher
pressure in the vessel H than in the condenser 5.
of it, from the water by contact with a water im
This system has the advantage that the solvent
miscible quinone solvent, separating the water
30 therefrom and returning it to the condenser.
need not be subjected to a high vacuum under
.As an example of this invention, quinone is ‘ which it would evaporate and be lost, or would 30
distilled from a reaction mixture by the use of have to be recovered in part through an expen
sive recovery system. A low boiling solvent is
steam and preferably under a vacuum, for ex
7 ample, such as to produce a temperature of the desirable in the subsequent recovery of the
quinone.‘ The chamber 15 may even be under
35 » order of 60 to 80° C. and the distillate condensed
in water from which the quinone is removed with pressure if desired. Thus, very low boiling sol
a quinone solvent so that the quinone content of
the water is kept so low that there will be no
blocking of the condenser and no cake will be
40 formed on the pipe leading into the water.
This result may be accomplished by discharg
ing the quinone vapors beneath a body of water
_Which is then circulated rapidly into another
chamber and then passing it through or in con~
tact with a solvent, and returned to the con
vents may be employed.
The water in the condenser 5 should be kept
slightly acid to prevent decomposition of qui
none. The water may be cooled by vacuum in
duced evaporation.
Any water immiscible solvent may be employed,
but preferably it should be one having a high
vapor pressure'wherever heat or a high vacuum
is employed.
The quinone may then‘ be recovered readily
The rapidity of circulation ‘and the volume of from the solvent and the water.
Water are, of course, adjusted so that caking is
The invention is, of course, applicable to any
entirely or substantially prevented. These ad
other compound, organic or inorganic, which
justments will, of course, also depend upon the _ has a tendency to cake in the condenser, and
solubility of quinone in the solvent.
which is volatile with steam.
densing vessel.
The invention is illustrated diagrammatically
in the drawing, in which i represents a still con- ‘
taining a reaction mixture 2 into which steam
65 may be supplied by the line 3. The reaction mix
The foregoing detailed description has been
given for clearness of understanding only and
no unnecessary limitations should be understood
therefrom, but the appended claimsshould be
2,136,966 '
construed as broadly as permissible in view of
the prior art.
I claim:
1. The method of distilling a. quinone which
comprises volatllizlng the quinone with steam,
condensing the vapors in a body of water in the
substantial absence of an organic solvent for
the quinone, and continuously extracting the
qulnone from the water by circulation of the
10 water through a body of solvent to maintain the’
concentration of the quinone therein at a point
so low that it will not form a cake in the con
2. The method as set forth in claim 1, in
which the water is cooled by maintenance of a
vacuum thereon.
3. The method as set forth in claim 1 in which
the quinone is benzoquinone.
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