Process and Plant for Separating Ammonia from a Gas Mixture
Field of the Invention
This invention relates to a process and a plant for separating ammonia from an ammonia-containing gas mixture by mixing the gas mixture with an aqueous liquid by which the ammonia is at least partly absorbed.
Prior art
Such processes and apparatuses are known per se. One important use thereof consists in the processing of gas condensate obtained in the fixed-bed gasification of coal by the Sasol-Lurgi process. In this processing tar, oil, phenols one after the other and subsequently acid gas and ammonia are separated from the gas condensate one after the other. These processes are described in GASIFICATION, 2nd Ed., Christopher Higman/Maarten van der Burgt, Gulf Professional Publishing, Chapter 5.1.1 and in Ullmann's Encyclopedia of Industrial Chemistry, 6th Ed., Vol. 15, Chapter 6, page 430 ff.
In practice, the separation of ammonia frequently is carried out by absorption of the ammonia in an absorption column. The ammonia-containing gas mixture flows through the column from bottom to top and is guided through one or also several, e.g. three, packed beds. In counterflow thereto, water as absorbent is guided through the packings from top to bottom. In the bottommost packing, in which the
ammonia-containing gas mixture first gets in contact with the aqueous absorption liquid, the aqueous absorption liquid is circulated via one external heat exchanger each because of the large amount of ammonia absorbed at this contact and to dissipate the related large amount of absorption heat. This measure frequently also is carried out for the second packed bed.
As the absorption capacity of the aqueous absorption liquid always decreases with increasing temperature, it is required to keep the temperature increase caused by the absorption of the ammonia low by a correspondingly large amount of liquid. However, this leads to the fact that in the region of the bottommost packed bed, which first gets in contact with the gas mixture, the column must be designed with a very large diameter, in order to be able to uniformly distribute the large amount of liquid over the packed bed. This large amount of liquid to be circulated leads to large apparatus dimensions and corresponding costs which lower the economy of the process.
It is the object of the present invention to provide an improved process and a plant operating by this process, in which the contact between the ammonia-containing gas mixture and the absorption liquid is carried out in a less bulky and hence less expensive apparatus.
Description of the Invention
The object is solved by the invention according to claim 1 by a process for separating ammonia from an ammonia-containing gas mixture by mixing the gas mixture with an aqueous liquid by which ammonia is at least partly absorbed, wherein the gas mixture and the aqueous liquid are separately introduced into the inlet hood of a tube bundle heat exchanger and are mixed therein to obtain a two- phase gas-liquid mixture, wherein subsequently the gas-liquid mixture is passed through the tubes of the tube bundle heat exchanger, wherein the gas-liquid mixture is cooled by a cooling medium guided on the shell side, the gas-liquid mixture from the heat exchanger subsequently is transferred into a separator for separating the gas and liquid phases, wherein a gas phase depleted of ammonia
and a liquid phase enriched in ammonia are obtained and each discharged from the separator 18 for the further use.
According to the invention, mixing of the ammonia-containing gas mixture coming from the total stripping column with the aqueous liquid, the absorption of the ammonia and the dissipation of the absorption heat are carried out in a tube bundle heat exchanger. The gas mixture and the aqueous liquid are separately introduced into the inlet hood of the tube bundle heat exchanger and mixed therein to obtain a two-phase gas-liquid mixture, wherein subsequently the gas- liquid mixture is passed through the tubes of the tube bundle heat exchanger, wherein the gas-liquid mixture is cooled by a cooling medium guided on the shell side. Due to the fact that the ammonia-containing gas mixture and the absorbing liquid jointly flow through the tubes of the heat exchanger, the absorption heat in part is dissipated directly during its generation, the temperature increase of the liquid is lowered, and hence the absorption capacity of the liquid is increased. Subsequently, the gas-liquid mixture is transferred from the heat exchanger into an apparatus for separating the gas and liquid phases.
Preferred Aspects of the Invention
An expedient aspect of the invention consists in that the aqueous liquid is introduced into the ammonia-containing gas mixture by means of at least one nozzle in the inlet hood of the tube bundle heat exchanger. This is a simple method for uniformly distributing a liquid in a gas. One variant of the invention consists in carrying out the absorption of the ammonia in a multistage process, wherein the first stage is effected according to claim 1 or 2 and then, in a second stage, the obtained gas phase depleted of ammonia is passed into an absorption column and flows through the same from bottom to top, and wherein fresh water is introduced into this column, which flows through the column from top to bottom in counterflow to the gas phase, and wherein the gas depleted of ammonia is discharged from the column for the further use, and wherein the water loaded with ammonia is discharged from the
column as aqueous liquid and used in the first step, in that it is introduced into the inlet hood of the tube bundle heat exchanger.
By this measure, residual contents of ammonia are removed from the gas phase in a conventional way, i.e. by contact of the gas and liquid phases in one or several packed beds. In connection with the mixing of the gas phase and the aqueous liquid in the tube bundle heat exchanger according to the invention, particularly high degrees of separation can be achieved for ammonia with a generally small size of the apparatuses used.
Another particular aspect of the invention is characterized in that the absorption column used in the second stage is equipped with two separate, superimposed mass transfer devices, for example packed beds or structured packings, wherein the aqueous phase is circulated via the lower packing and for cooling guided over a heat exchanger located outside the column. This aspect is particularly advantageous when, according to the prior art, the absorption in the first step is carried out in a packed bed.
In a further aspect, the invention also relates to a ptant for separating ammonia from an ammonia-containing gas mixture, comprising the following plant sections:
(a) a tube bundle heat exchanger 16 with feed conduits for an ammonia- containing gas mixture 1 ' and an aqueous liquid 14 and a discharge conduit for a two-phase gas-liquid mixture 17', suitable for mixing the gas mixture 1' and the aqueous liquid 14 to obtain the two-phase gas-liquid mixture 17', and for cooling the same,
(b) a separator 18 provided downstream of the plant section (a) for separation into a liquid phase 12' enriched in ammonia and a gas phase 19 depleted of ammonia,
(c) an absorption column 2' provided downstream of the plant section (b) with respect to the gas phase, containing a feed conduit for fresh water 6', a discharge conduit for water loaded with ammonia as aqueous liquid 14, a discharge conduit for gas 13' depleted of ammonia and at least one mass transfer device 4', wherein a first part of the aqueous liquid 14 is delivered over a heat exchanger 10' by
means of a delivery device 8\ is cooled there and subsequently charged to the absorption column 2' above the mass transfer device 4', and wherein a second part of the aqueous liquid 14 is recirculated to the plant section (a). Exemplary embodiment
Further developments, advantages and possible applications of the invention can also be taken from the following description of exemplary embodiments and the drawings. All features described and/or illustrated form the invention per se or in any combination, independent of their inclusion in the claims or their back- reference.
In the drawings:
Fig. 1 shows a process for separating ammonia from a gas mixture containing ammonia and inert gases according to the prior art,
Fig. 2 shows an exemplary embodiment of the process according to the invention.
First of all, the prior art will be explained with reference to Fig. 1. The ammonia- containing gas mixture 1 is introduced at the bottom of the absorption column 2 and flows through the mass transfer devices 3, 4 and 5 one after the other, which here are designed as packed beds. Into the top of column 2 demineralized water 6 is introduced as absorbent and flows through the packed beds one after the other in counterflow to the ascending gas mixture. For the lower and middle packed beds 3 and 4 the water is pumped over by means of the pumps 7 and 8. Via the heat exchangers 9 and 10 the absorption heat generated during the absorption of ammonia is withdrawn from the water. In this way, a higher absorption of ammonia by the water is achieved. At the bottom of the column 2, aqueous liquid 12 enriched in ammonia is withdrawn via the pump 11 for the further use. At the top of the column 2 gas 13 depleted of ammonia, inert gas substantially containing nitrogen, is withdrawn for the further use.
Due to the large volumetric flow rates of the partly loaded absorbent, in particular the bottommost packed bed 3 must be designed particularly large. This results in large sizes for the absorption column 2 in particular with regard to the column cross-section. This in turn leads to increased investment costs and limitations with regard to the erection of the absorption column 2 wirthin the plant complex. Furthermore, the pump 7 and the heat exchanger 9 must be designed correspondingly powerful.
As an example for a design of the process according to the invention, Fig. 2 shows how the ammonia-containing gas mixture 1 ' and a stream 14 of aqueous liquid are introduced into the inlet hood 15 of a tube bundle heat exchanger 16. After it has flown through the tubes of the heat exchanger, wherein a large part of the ammonia from the gas phase has been absorbed by the liquid phase and absorption heat has been dissipated, the resulting two-phase gas-liquid mixture is introduced as stream 17' into a separator 18 for separating the gas and liquid phases. From there, the gas phase is introduced into the bottom of the absorption column 2' as stream 19 and flows through the packed beds 4' and 5' to the top of the column 2'. At the top of the column 2' demineralized water 6' is introduced, which as absorbent takes up residual contents of ammonia from the gas phase. The gas phase largely liberated from ammonia leaves the column 2' at the top as stream 13' for the further treatment. Via the lower packed bed 4' the water is circulated by means of the pump 8', wherein absorption heat is dissipated via the heat exchanger 10'. From the circuit, the stream 14 is branched off towards the heat exchanger 16. The generated aqueous liquid 12' enriched in ammonia is discharged from the separator 18 and supplied to the further use by means of the pump 11 '.
Industrial Applicability
The invention represents an inexpensive alternative to a practically employed process and therefore is commercially applicable.
List of Reference Numerals
1 , 1' gas mixture, containing ammonia
2, 2' absorption column
3 mass transfer device
4, 4' mass transfer device
5, 5' mass transfer device
6, 6' fresh water or demineralized water
7 pump
8, 8' pump
9 heat exchanger
10, 10' heat exchanger
11 , 11' pump
12, 12' aqueous liquid, enriched in ammonia
13, 13' inert gas, depleted of ammonia
14 aqueous liquid
15 inlet hood
16 tube bundle heat exchanger
17' gas-liquid mixture
18 separator
19 gas phase