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Патент USA US2407823

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Sep@ 37» E946.,
Filed Dec. 14, 1943
Patented Sept. l?, i946
es “E
A ¿£107,822
sono associare
Frank C. Fahnestock, Haddoniield, N. Il., and>
William A. Hagerbaumer, Haverford Township,
Delaware County, Pa., assignors to Socony
Vacuum @il Company, incorporated, a corpora
tion oi New York
~application December le, i943, Serial No. 514,222
s ois.
This invention has to do with the making of
various acid reagents utilizing the oxides or sul
For example, in sulfonation processes, it is fre
quently desired to use solutions of sulfur triox
ide in liquid sulfur dioxide, or oleum of quite high
This inventionl is directed to a convenient and
highly efficient method for handling the prepa
ration >of many such reagents.
The invention may be understood by reference
to the attached drawing, the single figure of
which shows, in. diagram form, apparatus appro
priate to carrying out the invention, which may
be operated as follows:
Turning to the drawing, i is a stripper tower.
having a fractionating section 2 and an exhaust
ing section 3. An oleum, say one containing 20 %
(ci. 2aB-irri
shown, other types of equipment useful for the
absorption oi’ gases in liquids may be used.
Working in another Way, the operation can be
utilized for the producing of strong oleum from
relatively weaker oleum. Still introducing 20%
oleum through pipe ll to the stripper l and de
nuding it of sulfur trioxide to produce a denud
ed 3% oleum, the 20% oleum may be introduced
into absorber I6 through pipe 26 and spray 2l.
10 In this operation, under control of absorber con
ditions effected in the usual manner by the tem
perature of the entering oleum and system pres
sure as eiïected by control of gas vent 2d, any de
sired strength of oleum can be produced by con
15 trolled absorption of sulfur trioxide.
It will also be possible, operating in this Way,
for purposes where its use is desirable, as. in '
some sulfonation operations, to produce mixtures
_S03 is fed to this tower through pipe t, passing
of oleum and liquid sulfur dioxide.
through heater 5 and entering the tower through 20
As an example of the operation, working in
spray 6. The function of this tower is to strip
S03 from the oleum, and to this end there is
introduced, by pipe l and spray 8, a stream of
tower l at a feed temperature of 225° F. and a
pressure of 2 1b. gauge with a bottom tempera
ture of 250° F., a 15% oleum may be lstripped to
vaporous sulfur dioxide. This stream of gas may
a 3% oleum. The stripper overhead may then
be heated in heater 28. Control of tower con 25 be treated in absorber i6 at atmospheric pres
sure and a temperature of .l5-20° F. to produce
ditions is eil'ected in the usual manner by a wet
a liquid consisting of 80% by weight of sulfur
reilux of liquid sulfur dioxide, introduced from
pipe s through spray i0. Additional heat, as
dioxide and 20% by weight of sulfur trioxide.
necessary, may be supplied by reboiler il. Op
If oleum is used as the absorption agent, to pro
erating in this fashion, an oleum may be stripped 30 duce a stronger oleum, the working temperature
readily to a 10W concentration, say for example
of the absorber will usually be about 40° F. or
to one containing 3% S03, which denuded oleum
less, at atmospheric pressure.
may be removed from tower l through pump l2
Quite obviously. the method may also be used
and pipe i3, under the control of liquid level valve
for the strengthening of sulfuric acid of low con
i6. The overhead product of stripping tower l, 35 centration, such as for raising the concentration
departing through pipe l5, consists oi' a gas
of a 66° Baumé acid by solution of sulfur triox
eous mixture of SO2 and S03.
ide therein, and for similar operations.
Instead `of the fractionator type of equipment
We claim:
l. That method of handling acidic oxygen
shown, other types of stripper may be used, as,
for example, a film type of evaporator.
40 products of sulfur comprising contacting an
oleum containing dissolved sulfur trioxide with
This mixture ls introduced into absorber tower
lâ, below its packing Il, through spray I 8, hav
gaseous sulfur dioxide under temperature and
ing ñrst been cooled by passing through cooler
' 2S. Liquid SO2 is introduced at the top of tower
pressure conditions conducive to evaporation of `
sulfur trioxide from oleum to produce a gaseous
l@ from pipe i9, through spray 20, in amounts
. mixture of sulfur dioxide and trioxide and then
which may be controlled by liquid level control
in a separate region contacting said gaseous mix
valve 2i, or otherwise, if desired. There is col
ture with a liquid absorbent for said sulfur tri
lected in the bottom of tower l5 a liquid SO2
oxide selected from the group consisting of liquid
containing dissolved S03, which may be with
oxides of sulfur and hydrates of sulfuric anhy
drawn for use through pump _22 and pipe 23. 50 dride to absorb sulfur trioxide therein.
2. The method of claim 1 in which the liquid
Control _of conditions within the absorber tower
may be elîected in several ways, as by control of
absorbent used is liquid sulfur dioxide and the
the temperature of the entering liquid S03, and
product is liquid sulfur dioxide -containing dis
by pressure control elîected through the agency
solved sulfur trioxide.
of valve 2d on SO2 gas vent pipe 25 as a modifier 55
3. 'I'he method of claim 1 ln which the liquid
oi’ system pressure. Working in this fashion, any
absorbent used is an oleum and the product is a
stronger oleum.
desired mixture of liquid sulfur dioxide and dis
solved sulfur trioxide can be achieved.
Instead of the fractionator type of absorber
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