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Патент USA US2125905

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Aug. 9, 1938‘.
M. R. FENSKE ET AL
2,125,905
PROCESS OF SEPARATING A MIXTURE OF TRIMETHYLAMINE AND AMMONIA
Filed March 3, 1937
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Patented Aug. 9, l9‘38
2,125,905
UNITED STATES PAT'EN 1' oFFIcE
,
2,125,905
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'.'rnncns's. or snrann'r'ma A mx'runn or
..
I .. Me'mufa. Fenlk'e'," suite ‘calm,
P
" Andrews, j Over-brook,
v1t: Haas Company.
' -,'Application:_Mai-cii.3,'
'
.
"and
‘
I
Philadelphia-Pa“
arassin
'
i937, sen-1 No. “128,140”
(or. ‘260-127) “
This invention relatesfto ‘me-process 6r manu superatmospherici pressure and theractual pres
lecturing methylamines' and particularly to" a I sure
used willnbe chosen so asv to, permit the con
process \for fractionally separatingiw-them lfrom‘
densatio'n ofithe, overhead gas to takeplacewitb‘
each other and from ammonia. ' ‘
5
. 1nv thejsystem and within the temperature range‘
‘ In the process ‘of producing‘the‘methylamines
.of available coolinglwater._ Variations in pres
from methanol and ammonia catalytically, the .'
sure‘h'ave onlya veryslight eil'ect on} the em‘
product contains all three methylamines, mono-p1" ioiency,
of- "the separation. '
f v
g,
di- and tri-, as well‘ as water and, the unreacted
_
ammonia and methanol. ' Ondistillation' the tri
10
'
'1] > The process'may be carried out many suitable
apparatus‘. such-as is shown in'the ‘drawing at
methylamine forms-a constant boiling mixture ' tached hereto. ‘The gas mixtureto- be separated
10
with ammonia and also with mono-methylamine. may
be bubbled ‘through the liquid in an appa-:
‘ so that it is impossible‘ to separate these materials
ratus'
such
as
isfshow'n
in
Figure
.1,»
or
it
may
be
completely by distillationruif'ltv is possible to re
run countercurrent to the liquid in'an apparatus
move allthe trimethylam'i'ne Ironiqthe"n1lxture,5_
N15 as a. constant boiling mixture,i'provided'suil‘lcient'
ammonia ‘is present‘,
V-as'showninFlgure 2;
.then'ito-separate the
except by ‘chemical means. i
,
It "is an object of‘this invention to provide a
method whereby the constant boiling vmixture of
trimethylamine and ammonia may be separated
completely into its individual components with
'-;
-
1'
Referring to the drawingandspeci?cally to 15.
'_mono- andv dimethylamines': ebyqordinary frac- '
ti'onaldis'tillation. In‘ this way
V
v‘pure vmonometh-' r
ylamineland pure 'dlrnethylamiue‘ could be pre-. '.
20 _ pared butit was impossible to separate the tri
methylaminein a pure'state from the ammonia
25
s
Figure 1, a cylindrical vessel-2' having a pipe 3
attached to the bottom, an inlet pipe _-4 and out
letvpipes' 5 and 5, is mounted ina jacket ,1 which completely surrounds the‘ vesselv 2'and lower ex
tension}, The jacket has an inlet pipe 8 and
an outlet. pipe 9.' A valve ity is inserted ‘in, the
inletp'fpe 9 to control the ?ow of heating or cool
ing liquid to the Jacket. Thermocouples or ther
mometers II and I2 are/inserted in the inlet and
outlet pipes respectively, to record. the tempera
ture of the heating or cooling liquid. A pipe l3
out causing‘ any chemical changes to take place. ‘ with valve I4 is connected to the ‘inlet pipe I of
The present invention is based on- the'fact that the inner vessel and a valve I5 is attached to- an
the solubilities of trimethylamin'e and ammonia extension
of inlet pipe I." The outlet pipe 5 has
30 in any’ given solvent‘ are different, and by suit
a valve ii to control the ?ow of solution from the
ably arranging the relative amounts‘ of solvent inner vessel. The. outlet pipe 6 also has 'avalv'e
and gas mixture fed into the system in a given
I‘! to control the flow of gas from the inner vessel
time, a complete separation or the tvid‘can be
' and a pressure gage l8 for recording the‘pressure
attained.
1:15
,
'
The mixture of trimethylamine and ‘ammonia
does not ‘have to correspond in composition to
the constant boiling mixture, since any mixture
of the two can be saparated in this manner.
In
the examples chosen to illustrate this invention
40 a mixture approximating that of the constant
boiling mixture is used,’ for the reason that such
mixtures are met with more‘ frequently in the
process of manufacturing methylamines. The
liquid used for the separation of the .two com
ponents will determine which of the two remains;
in solution, the other being removed in the'gas
eous “ form and subsequently condensed.
eter I9 is inserted in the inner vessel 2’ to show 35
the temperature of the liquid.
'
Figure 2 shows a di?erent apparatus for carry
ing out the same process. _An" inner tube 2| is
surrounded by a jacket22. This jacket vhas an
inlet pipe 23 and an outlet pipe 24 in which are
inserted thermocouples ‘or ‘ thermometers 25 ' and
26 for recording ‘the temperature of the heating
?uid. A valve 21' inthef'inlet line ‘controls the
?ow of this ?uid.
_
.
.
'
, Y
"
The inner tube has‘ a lower extension 28 to
which an inlet pipe 29 carrying a'reg'ulating valve
When ' 30 and a pressure gauge'3l,‘ is attached: The
water is used for the separation, the ammonia
will remain in the water and the amine will be
50 removed as a gas.
within the vessel 2. A thermocouple or thermom
If an organic solvent, such '
as triisobutylene, or a petroleum fraction, such
as gasoline, kerosene, gas oil or even ‘lubricating
oil, is used, the ammonia will pass through‘as
a gas, leaving the amine dissolved in the liquid.
55
The process is preferably carried out under
lower extension 2_8‘also"carries a sight- glass 32
and a valve 33 for regulating
from the‘inner tube.‘v An inlet
35 are attached to the upper
tube as are the outlet‘ pipe 35
the ?ow of liquid
pipe 34 and valve
end of the inner
and valve 31.
In operating the apparatus‘ shown in Figure 1,
water or other heating medium’ at any desired
temperature is’ passed continuously through the
9,195,905
.2
Jacket. In order to assist in maintaining the
temperature the jacket may beinsulated it de
sired.
-
-‘
'
-
The inner vessel is nlled'with water or other
liquid to the level L so that it will just over?ow
through pipe 5. The trimethylamine and am
monia to be separated are then admitted through
valve ll and by keeping valve I‘! closed, any
desired pressure up to the saturation’pressure or
the invention may be otherwise practiced within
the scope of the appended claims.
Example 1.--'I'he same gas mixture as in pre- ‘
vious examples was charged to the apparatus
shown in Figure 2. The temperature of the water
entering the jacket was 93° F. and at the outlet
was 118° F. The pressure within the tube was
30 pounds per square inch. Triisobutylene was
used as the absorbing liquid and was fed at a rate
Valve I1 is then _ of 0.47 pound per hour.
the solution may be attained.
The gas mixture was
keep the pressure reasonably fed at 0.23 pound per hour of which 0.074 pound
or 32% was absorbed, the remainder passing
constant. ,By regulating valves lland I‘ a con
stant ?ow of liquid can be maintained through "through the system. The overhead gas contained
7% trimethylamine and 93% of ammonia or 10%,
' opened enough to
the apparatus.
16
.
As the mixture of gases passes through, the
more soluble one is concentrated in the liquid
and the less soluble one passes through and is
removed through valve l1 .
_
'
Alter the apparatus is in operation the flow
of liquid and’ gas mixture are set at constant rates
which results in a constant degree of separation
of the components of the gas.
‘
The apparatus shown in Figure 2 operates some
what di?erently. The inner tube It is packed
with any ordinary tower packing such as rings,
chains, broken tile, etc. Bubble .plates may also
be used if desired. Water or other heating or
cooling ?uid is passed through the jacket so as to
maintain the desired temperature within the inner
30 tube II. The gas mixture is admittedv at a con
stant rate through valve Ill and when the desired
pressure is attained it is regulated by proper ad
iustment of the exit valve 31. Water or other
absorbing liquid is admitted through valve 35
and pipe 34 and trickles down over the pack
ing through the sight glass 32 and is drawn of!
through valve 33.
As the gases and liquid pass in opposite direc
tions the more soluble one is removed by the liquid
40 and the less soluble one passes out through valve
31. Alter the apparatus is in operation the rates
of how of gas and liquid are kept constant so that
a constant degree of separation of the compo
nents of the gas is attained.
The pressure and temperature may be varied
45
over a considerable range without a?ecting the
emciency of the separation. It is even. possible
to adjust them so that two liquid phases are pres
and 38% respectively of the total amounts ted to 15
the system.
Example 2.-Kerosene was substituted for the
triisobutylene and was led at the rate of 0.49
pound per hour. Thelsame gas mixture as previ
ously was fed at the rate of 0.17 pound per hour 20
of which 0.034 or 20% was absorbed. The over
head gas contained 3% oi! trimethylamine and
97% of ammonia and the gases contained in the
liquid contained no ammonia. In this case prac
tically a complete separation oi.’ the two gases 25
was obtained on a single pass through the appa
ratus.
This application is a continuation-in-part of
copending application Serial No. ‘748,476- ?led
_October 16, 1934 which has matured into U. S. 30
Patent #2,091,630.
-We claim:
.
1. The process of separating a mixture of tri
methylamine and ammonia which comprises se
lectively absorbing the trimethylamine in an all
ture in contact with a stream of said solvent ?ow
ing countercurrent thereto.
2. The process of separating a mixture of tri
methylamine and ammonia which comprises se 40
lectively absorbing the trimethylarnine in kero
sene by passing the mixture in contact with a
stream of kerosene ?owing countercurrent there
3. The process of separating a mixture of tri
methylamine and ammonia which comprises se
lectively absorbing the trimethylamine in an all
phatic hydrocarbon solvent.
4. The processor separating a mixture of tri
methylamine and ammonia which comprises se
The
following
examples
will
serve
to
illustrate
50
the operation of both types of apparatus but the’ lectively absorbing the trimethylamine inxkero
invention is not limited to the exact conditions of
MERRELL R. FENSKE.
temperature, pressure, rates of ?ow or composi- ‘
CHESTER E. ANDREWS.
tion or the gas mixture given in the examples, as
ent in the inner tube.
85
phatic hydrocarbon solvent by passing the mix
‘
sene.
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‘
50
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