Patented Sept. 19, 1922.

, 1,429,483

UNITED‘ STATES PATENT OFFICE.

CARL BOSCH AND WILHEIM MEISER. 0F LUDWIGSHAFEN-ON-THE-RHINE, GERMANY, ,
ASSIGNORS. BY MESN E ASSIGNMENTS, TO BADISCHE ANILIN & SODA FABRIK, OF
LUDWIGSHAFEN-ON-THE-RHINE, CBAVAZRJIIA,v GERMANY, A CORPORATION OF THE
GRAND DUCHY OF BAIDEN.
PROCESS OF MANUFACTURING UREA.

No Drawing. Application ?led July' 9, 1920.‘ Serial No. 395,149.

To all whom it ’llb(l~_l/ concern: hours. Then the reaction mass, being un
Be it known that we, CARL Boson and der pressure of from about 50 to 100 atmos 55
\VILi-inLu Mnisnn, citizens of Germany, re pheres dependin on the temperature of the
siding at Ludwigshafen-on-the-Rhine, Ger reaction mass, is slowly released through
5 many, have invented new vand useful Im a bottom valve into a distillation appara
roveinents in Processes of Manufacturing tus, e. g., a column, in which the unaltered
llrea (for which I have made application starting material is expelled in the form 60
in Germany, Aug. 9, 1916; in Austria, July of a mixture of carbon dioxid and am
14, 1917; and in Hungary, July 21, 1917), monia, partly by the heat of the melt it
10 of which the following is a speci?cation. self, partly by heat introduced into the col
The present invention relates to an im umn, e. g., by introducing steam from be
proved method of manufacturing urea. We low, whilst a solution of urea, practically 65
have found that. the production of urea free from ammonium salts,‘ runs off from
from carbon dioxid and ammonia can be ef the bottom. The column is preferably pro
15 fected in a simple manner by forcing the vided with a dephlegmator and the mixture
mixture of the two gases in about the pro-' of ammonia and carbon dioxid escaping
portions required according to the equation from it is directly drawn off by the coin 70
pressor and again forced into the autoclave.
Q‘NH3+CO2:CO(NH,)2+H2O The compressor and connection pipes are
20 into a vessel capable of withstanding the su?iciently preheated to avoid precipitation
pressure and maintaining the melt of am of liquid, or solid, ammonium carbamate
monium salts formed, at the temperature or carbonates. In order to replace the 75
suitable for the transformation of ammo starting material withdrawn by the forma
nium-carbamate into urea say from about tion of urea, either fresh carbonic acid and
25 130 to 1-10 degrees centigrade introducing ammonia may be forced into the autoclave
as much additional heat as may be found separately, or together, or, more simply, an
necessary. The compression and convey aqueous solution of ammonium carbamate, 80
ance of the mixed ammonia and carbon di or carbonate, may be introduced into the top
oxid is rendered possible, according to the [part of the column, which solution can be
30 invention. by keeping the compressor and prepared in a separate vessel from carbon
the pipe connections at a temperature suf dioxid and ammonia and an impure carbon
licieutly high to avoid the separation of dioxid may be employed therefor. The 85
liquid or solid ammonium carbamate, or proportion of moisture contained in the mix
carbonates. By this process the separation ture of ammonia and carbon dioxid to be
35 of ammonium carbamate in a solid, or carried back through the compressor may be
liquid, state becomes unnecessary, and it is controlled by maintaining a suitable tem
even possible to work continuously. In or perature at the outlet of the dephlegmator, 90.
der to obtain this result, the reaction mass, e. g. that of 60 degrees centigr. is chosen.
after urea has been formed, is slowly dis As a large quantity of water is detrimental
40 charged, while maintaining the pressure in to the formation, of urea the amount of
the vessel, and the mass withdrawn is sep moisture should be kept small and at any
arated while lowering its pressure, into a rate below that required‘ for the formation 95
solution of urea and a gaseous mixture of of ammonium'carbcnate, according to the
ammonia, and carbon dioxid, which mixture equation
45 is again compressed and forced back into the
vessel. '
For example, the process is carried out. in The expansion of the melt may also take 100
the following manner. -A suitable mixture place, in order to save compression energy,
of carbon dioxid and ammonia, preferabl ?rst down to an intermediate pressure, say
50 in a somewhat moist condition, is force , 10 atmospheres, at which a part of the car
by means of a preheated compressor, into bon dioxid-ammonia mixture distils off ‘and 1~
an autoclave and the melt obtained kept is directly led, for instance, to the second 105
at about 135 degrees centigr. for say two stage of the compressor, whilst the rest will
 1,4221%48e
vaporize after the complete expansion in suitable for effecting the formation of urea, 40
the column and is carried to, the ?rst stage continuousl withdrawing part of the reac
of the compressor. 2 tion mass a ter urea has been formed, lower
We claim : ing the pressure of the mass withdrawn,
1. The process. of manufacturing urea separating it into urea solution and a gase
which consists in compressing a mixture of ous mixture of ammonia and carbon dioxid, 45
ammonia and carbon dioxid in about the which mixture is again compressed and car
proportions required for the formation of ried back to the ?rst-named melt, while
- urea while said mixture is kept during com maintaining the gaseous mixture during
.10 pression at an elevated temperature to avoid compression and conveyance at an elevated
the separation of ammonium salts, convey temperature to avoid the separation of 50
‘ ing the compressed gaseous mixture while liquid or solid ammonium salts.
maintaining said temperature, then reduc 4. The process of manufacturing urea
ing it to a melt by lowering the tempera which consists in maintaining a melt of am
315 ture and maintaining the melt. at a tempera monium salts, which is formed from a mix
ture suitable for effecting the formation of ture of ammonia and carbon dioxid in about 55
urea. the proportions required for the formation
‘ 2. The process of manufacturing urea of urea and in the presence of a small
' which consists in maintalning a melt of amount of water below that contained in
ammonium salts, formed from a mixture of ammonium carbonate, under pressure at the -
ammonia and carbon dioxid in about the temperature suitable for effecting the for 60
proportions required for the formation of mation of urea, continuously withdrawing
urea, under pressure at the temperature suit part of the reaction mass after urea has
able for effecting the formation of urea, been formed, lowering the pressure of the
@6 withdrawing the reaction mass after urea mass withdrawn, separating it into urea
has been formed, lowering the pressure of solution and a gaseous mixture of ammonia 65
the mass withdrawn, separating it into urea and carbon dioxid by heating, which mix
solution and a gaseous mixture of ammonia ture is then again compressed and carried
and carbon dioxid, which mixture is again back to the ?rst-named melt which is con
compressed to form a melt while maintain ' tinuously kept under pressure, while remov
ing it. during compression and conveyance ing from the gaseous mixture part of the 70
at an elevated temperature to avoid the sep moisture and maintaining it during com
aration of liquid or solid ammonium salts. pression and conveyance at an elevated tem
3. The process of manufacturing urea perature to avoid the separation of ammo
86 which consists in maintaining a melt of nium salts.
ammonium salts, formed from a mixture In testimony whereof we have hereunto 75
of ammonia and carbon dioxid in about the set our hands.
proportions required for the formation of CARL BOSCH.
urea, under pressure at the temperature WILHELM OMEISER.