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Патент USA US2277115

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Mar¢h24,1942.1
H, KRUGER HAL
„
‘
-2,277,115
_ PROCESS FOR PRGDUCING PURE BENZENE HYDROCARBONS
‘Filed Aug. 4, 1938
' 2 sheets-sheet 1.
5MM
/
ATTORNEY.
` March 24, 1942.
H. KRUGER ETAI..
' 2,277,115
PROCESS FOR PRODUCING PURE BENZENE HYDROCARBONS
File‘d Aug. 4, 1938
5ÈS8%
...fr.Ü
2 'sheets-sheet 2
2,277,1_15
Patented Mar.V 24, 1942
’a UNITED STATES. PATENT orifice`
2,277,115
` A
PROCESS FOR PBODUCING PÚRE BEÑZENE
' »
HYDBOCARBONS
Hugo Krüger, Gottesberg, Kreis Waldenburg in
Schlesien, and Kurt Gieseler, Hermsdorf, Kreis
Waldenburg in Schlesien, Germany, assignors`
to Sherka Chemical Co. Inc., Bloomlield, N. J., a '
corporation of> New York
Application August 4, 193s, sei-m No. 223,07
In Germany August 5, 1937
comms. _ (ci. 2oz-c7)
This invention relates to a. process for the'
manufacture of pure hydrocarbons of the ben
zene series.
In order to produce pure benzene, pure toluene, “C
invention and by selection of a suitable com
position of the starting material, there is ob
tained in a continuous distillation operation with
out any intermediate fractions, in the form of
standard pure hydrocarbon, 90~95% of the, pure
hydrocarbon present in the starting material.
pure xylene or other hydrocarbons of the benzene
series in general'one has hitherto proceeded in
The invention is described below with refer
such a manner that the crude or puriñed benzene,
' ence to the‘accompanying drawings which illustoluene or xylene fractions obtained by frac
trate diagrammatically arrangements of stillsA
tionation, after washing with concentrated sul
phuric acid, were subjected to a very careful dis w for carrying out the present process in-which
continuous distillation which was finally carried
like reference characters indicate like parts.
out in horizontal stills which were providedwith
Fig. 1 is a diagrammatic view of any apparatus
-high columns. There are thereby always pro
adapted for carrying 'out the p'resent process, and
Fig. 2 is a similar view showing a modified ap
duced considerable quantities of intermediate
fractions, first and after runnings so that the
paratus for carrying'out a modiñcation of the
present process.
. _
yields of pure hydrocarbons did not amount to
more than 80%.
Continuous distillation for the production of
motor benzol has heretofore been _carried outin
'
Referring to Figure 1, the crude product,
washed with caustic soda lye and sulphuric acid,
is preheated and introduced at a into the column
such a manner that with removal of an initial 20 I to about _1/2 to 2A, of the height. The column l
contains fractionating coils divided into two sec
fraction and a residual fraction, an intermediate
usable motor benzol with boiling limits of 80
tions, which-in the bottom part are heated with
steam, and consist to the extent of 1/2 to 2A; of
been possible by means of continuous distilla
vaporizing coilsand tothe extent of 1/3 to 1/2 of
tion of light oils to obtain toluene almost quan 25 rectifying coils. In this column all constitu
titatively in the form of crude or purified toluene
ents b boiling lower than the hydrocarbon to
with boiling limits of 10G-120° C.
be produced are distilled ofi and the hot residue c
leaving the column 1' through a pipe is con
Hitherto, however, it has not been possible, on
a commercial scale by means of continuous dis
tinuously delivered by. means cf the pump P to
tillation in a progressive distillation operation 30 the column 2. The column 2 contains as many 4
and without the occurrence of intermediate frac
or imore rectifylng coils than vaporizing coils so
tions to obtain pure hydrocarbons such as
thatv the pure hydrocarbon d distils oiî within
the required boiling limits and is separated from
Pure benzene, boiling to the extent of 90%
within 0.6° C. and to the extent' of 95% within
the residue which leaves at r.
85 In order to attain in the column I the com
0.8° C.,
.
.,
plete separation of all constituents boiling lower`
Pure toluene, boiling to the extent of _90%
than the pure hydrocarbon to be produced, the
within 0.6° C. and to the extentvof 95% \within
0.8° C., or
'
'
_
i
liquid residue flowing oif from the column must
Pure xylene, boiling to the extent of 90%
have a boiling point which in the case of pure
within 3.6° C. and to the extent of 95% within 40 benzene manufacture amounts to at least 86° C.
4.5" C.
and in the case of the manufacture of pure
It is true that the Kubierschky column ha
toluene amounts to at least 115° C., that is to say
been recommended for the continuous separation
about 5° C. above the boiling point of the pure
hydrocarbon to be produced. If this isl not the
of benzene, toluene and xylene (Lunge-Köhler,
“Die Industrie des Steinkohlenteers und des 45. case then the lower boiling constituents cannot
Ammoniaks" vol. 1, 1912, Page 897); there is. ' be distilled off .without residue and the lower
boiling limit of the pure hydrocarbon to be pro
¿thereby obtained, however, from crudebenzene
ñrst a 90% commercial benzol (see in particu
duced is too low. It is necessary either to select
lar page 899 last paragraph) which must then
the composition of the starting material such
be worked up to pure benzene in a’ second dis 60 that for example the crude toluene boils to the
continuous distillation operation in which case
extent of 95% between 10D-130° C. and contains
at least 10% Xylenes or care must be takenl
the known intermediate fractions are produced.
In contradistinction to the above, by the ap
by the admixture of. higher boiling constituents
plication of the arrangement> and construction
that the residue from the ñrst column has the
of consecutive columns according to the present 55 necessary high boiling polntand is obtained from
. 150° C. has been obtained. Recently it has also
2
2,277,115
said residue, and condensing the pure vapors of
the lower part of this column as a liquid which
can be washed out.
' the desired hydrocarbon.
l
the required boiling point, or a puriñed toluene
2. A process for the production of a pure hy
drocarbon taken from the class consisting of
benzene, toluene, and xylenes from crude liquid
mixtures with other hydrocarbons of the benzene
series which comprises introducing into the recti
whichstill contains aconsiderable proportion of _
ilcation zone of a column such a crude mixture
If, however, for example it is desired to work
up a puriiled toluene which-boils to the extent
of 95% Within 10D-120° C. the residue of which
coming from the first column does not, exhibit
together with higher boiling hydrocarbon con
stituents, the latter being in sufiicient amount to
raise the boiling 4range of the mixture (after
the main columns in each case an auxiliary
vaporization of constituentsv boiling below said
column (Figure`2). Together with the column I
pure hydrocarbon) suiiiciently above the normal
thus the lateral column A is operated. To this
.boiling point of said pure hydrocarbon to sub
latter is supplied a deñnitely adjustable propor
tion e of the residue from the former column I, 15 stantially prevent distillation of said pure hydro
carbon during said vaporization, subjecting the
for example lil-20% of the original quantity a,
same _to the action of vaporizing and rectifying
which is withdrawn from one or more still sec
lzones in said column, causing vaporization of
tions, consisting of about y», benzene and %
substantially all of the lower boiling hydrocar
toluene and thus containing all the heptane.
bons untilthe liquid residue in said column has
This portion e is separated in the auxiliary col
parañn hydrocarbons such as` heptane or octane,
it has proved to be advantageous to attach to
umn A into benzene with heptane f and a con
a boiling range of atleast 5° C. above the boiling
siderably concentrated toluene, about 98%, g
point of the pure hydrocarbon to be produced, '
which is either mixed again> with the product
to be worked up i. e. the column ,I or employed
passing said residue into' a second column and
in some other way.
causing vaporization of said hydrocarbon from '
The distillates of the two 25 said residue, and condensing the pure vapors of
columns b and j are combined.
the desired hydrocarbon.
A
The liquid residue c from column I is >free
,
>
3. lA process for the production of a pure hy
drocarbon taken from the class consisting of
benzene, toluene, and xylenes from crude liquid
uously through the heater D into the column 2 -30 mixtures with other hydrocarbons of the benzene
series which comprises introducing into the recti-~
in which as distillate d pure toluene is obtained.
` flcation zone oi a column such a crude mixture
In the case of the presence of substances which
together with higher boiling hydrocarbon con
boil between toluene and xylene a certain~ pro
stituents, the latter being in suñicient amount to
portion h of the residue from the column 2 is
drawn oil' laterally from the still sections and 35 raise the boiling range of the mixture (after
from all constituents boiling lower _than toluene
and is forced by means of the pump P contin
supplied to the auxiliary column B in which as
‘ vaporization of constituents boiling below said
distillate i pure toluene is also produced while
pure hydrocarbon) suiilciently above the normal
boiling point of said pure hydrocarbon to sub
the residue is combined with that from 2. In
stantially prevent distillation of said pure hydro
this'manner there is obtained by means of the
carbon during said vaporization, subjecting the
continuous distillation, even in the case of work
same to the action of vaporizing and rectifying
ing up of crude toluene boiling between 100 and
zones in said column, the vaporizing zone being
120° C. or toluene containing paraiiin hydrocar
greater in extent than the rectifying zone, caus
bons, a pure toluene in a yield of over 90%.
ing vaporization of substantially all of the lower `
While we have herein shown and described cer
tain preferred embodiments of our invention, 45 boiling hydrocarbons untilthe liquid residue in
said column has a boiling range of at least 5° C'.
we wish it to be understood that we do not con
above the boiling point of the pure hydrocarbon
_tobe produced, passing said residue into a second
column and causing vaporization of said hydro
and variation may be made without departing
carbon from said residue, and condensing the
from the spirit of the invention or exceeding 50 pure vapors of the desired hydrocarbon.
fine ourselves. to all the precise details herein
set forth by'wayof illustration, as modification
thescope of theßappended claims.
What we claim is:
‘
4. A process for the production of a pure hy
.
drocarbon taken from the class consisting of
1. A process for the production of a pure hy
benzene, toluene, and xylenes from crude liquid
drocarbon taken from the class consisting of 55 mixtures with other hydrocarbons of the benzene
benzene, toluene, and xylenes from crude liquid
series which comprises introducing into the rec
mixtures with other'hydrocarbons of the benzene
series which comprises introducing into the rec
tincation zone of a 'column' such a crude mix
tiñcation zone-of a column such a crude mixture
together with higher boiling hydrocarbon con
stituents, the latter being in suilicient amount to
ture together with higher boiling hydrocarbon 60 raise the boiling range of the mixture (after
constituents, the latter being in suflìcient amount
vaporization of constituents boiling below said
to raise the boiling range of the mixture (after
purev hydrocarbon) suillciently above the normal
vaporization of constituents boiling below said
boiling point of said pure hydrocarbon to sub
pure hydrocarbon) sufficiently above the normal
stantially prevent distillation of said pure hydro
boiling point of said pure hydrocarbon to sub 65 carbon during said vaporization, subjecting the
stantially prevent distillation of said pure hy
, same to the action of vaporizing and. rectifying
drocarbon during said vaporization, subjecting
`zones in‘said column, the vaporizing zone being
the same to the action of vaporizing and recti
r fying zones in said column, causing vaporization
of substantially all of the lower boiling hydro
carbons until the liquid residue in said column'
has a boiling range substantially above the boil
ing point of the pure hydrocarbon to be produced,
passing said residue into a second column and
causing vaporization of said hydrocarbon from
greater in extent than the rectifying zone, caus
ing vaporization of substantiallyall of the lower
70 boiling hydrocarbons until the liquid residue in
said column has a boiling range at least 5° C.
above the boiling point of the~pureìhydrocarbon
to be produced, passing said residue into a second
column having yrectifying and vaporizing zones,
the rectifying zone being greater in extent than
A
3
2,277,115
‘the vaporizing zone, and causing vaporization of
said hydrocarbon from said residue, and con
densing the pure vapors of the desired hydrocar
_ bon.
5. A process for the production of pure benzene
from crude liquid mixtures thereof with other i
hydrocarbons of the same series which comprises
providing such a mixture together with higher
boiling hydrocarbon constituents, providing such
higher boiling constituents in sufficient amount
to raise the boiling range of said hydrocarbon
mixture sufiiciently above the normal boiling
.point of benzene to substantially prevent dis
tillation thereof during vaporization of lower
boiling constituents of said mixture, introducing
said mixture into the rectification zone of a co1
umn, subjecting the same to the action of va
6. A process for the production of pure toluene
from crude liquid mixtures thereof- with other
-hydrocarbons of the same series which comprises
providing such Aa mixture together with higher
boiling hydrocarbon constituents. providing such
higher boiling constituents in sufiici'ent amount
_ to raise the boiling range of said hydrocarbon
mixture sufficiently above the normal boiling
pointl of toluene to vsubstantially prevent dis
tillation thereof >during vaporization of lower
boiling constituents of said mixture, introducing
said mixture into the rectiñcation zone of a
column, subjecting the same to the ,action of
vaporizing and rectifying zones in said column,
causing vaporization of substantially all of the
lower’boiling hydrocarbons until the residue in
said column has a boiling range of at least 115°
C., passing said residue into a second column and
porizing and rectifying zones in `said column,l
`causing vaporization of toluene from said residue,
causing vaporization of substantially all of the
lower boiling hydrocarbons until the residue in 20 and condensing the pure toluene.
said column has a boiling range of at least 86° C.,
passing said residue `into a second column and
causing vaporization of benzene from said resi
due, and condensing the'pure benzene.
HUGO KRÜGER.
KURT GIESELER.
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