AU2015335275B2 - Process and plant for separating ammonia from a gas mixture - Google Patents

Process and plant for separating ammonia from a gas mixture Download PDF

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Publication number
AU2015335275B2
AU2015335275B2 AU2015335275A AU2015335275A AU2015335275B2 AU 2015335275 B2 AU2015335275 B2 AU 2015335275B2 AU 2015335275 A AU2015335275 A AU 2015335275A AU 2015335275 A AU2015335275 A AU 2015335275A AU 2015335275 B2 AU2015335275 B2 AU 2015335275B2
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AU
Australia
Prior art keywords
ammonia
gas
liquid
mixture
phase
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AU2015335275A
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AU2015335275A1 (en
Inventor
Martin MÜLLER-HASKY
Gert Ungar
Tatjana WIDERSCHPAN
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/12—Separation of ammonia from gases and vapours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/10—Inorganic absorbents
    • B01D2252/103—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/406—Ammonia

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Gas Separation By Absorption (AREA)
  • Treating Waste Gases (AREA)

Abstract

A process for separating ammonia from an ammonia-containing gas mixture (1') 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 (14) are separately introduced into the inlet hood (15) of a tube bundle heat exchanger (16) 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 (16), wherein the gas-liquid mixture is cooled by a cooling medium guided on the shell side, the gas-liquid mixture from the heat exchanger (16) subsequently is transferred into a separator (18) for separating the gas and liquid phases, wherein a gas phase (19) depleted of ammonia and a liquid phase (12') enriched in ammonia are obtained and each discharged from the separator (18) for the further use.

Description

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 outfor 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 twophase 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
WO 2016/062410
PCT/EP2015/025069 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 gasliquid 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 InventionyBg
An expedient aspect of the invention consists in that the aqueous liquid is y' ' / 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
WO 2016/062410
PCT/EP2015/025069 • 4 ·,; 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 tower 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. · / i
In a further aspect, the invention also relates to a plant 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 T 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
WO 2016/062410
PCT/EP2015/025069 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). / /
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 perse or in any combination, independent of their inclusion in the claims or their backreference. < / l· /> ϊ 7 0 ' y ?\ <
In the drawings: < < > / / - / - /-- 0
Fig. 1 shows a process for separating ammonia from a gas mixture containing ammonia and inert gases according to the prior art, 0 ·
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 ammoniacontaining 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. 0 /
WO 2016/062410
PCT/EP2015/025069
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 within 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 T 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'. ' / ./
WO 2016/062410
PCT/EP2015/025069
Industrial
The invention represents an inexpensive alternative to a practically employed process and therefore is commercially applicable. <
List of Reference Numerals
1.Γ gas mixture, containing ammonia
10 2, 2' · / / ' absorption column : . ^ :////
/ 3 / / / · mass transfer device :'< :7: < 777
4,4' // 7/ mass transfer
5, 5' 77 / / / / mass transfer device 7 / // //7 /<
6/6’ fresh water or demineralized water
15/ 77 7'7/ pump :· : /:
8; 8' :: pump / //'://7 7://yii./::::< / λ< :
9 77/7 heat exchanger 7 /: ·' :/7/7////
10,10' heat
11t11‘ '' pump ..:7//7 ///?// ./77::: 7:;
20 12, 12’ aqueous liquid, enriched in ammonia
13, 13r 7 : inert gas, depleted of ammonia
14 aqueous liquid 7 :: 7
15 7/ 7 7 inlet hood 77 /77: :/17
16 :7 tube bundle heat exchanger7/7 / //:
257 17' 7 /. : 7 7 gas-liquid mixture . 7 /:.: ./ / /
18 ::7 separator ' 7 7 7 / . .. /: ::
19 / · ' 7/ gas phase 7 ////:::/:; >< > :7/^ ///7 -:-//:''
WO 2016/062410
PCT/EP2015/025069
-/0--

Claims (6)

  1. Claims: / · /
    1. A process for / separating ammonia ' from an ammonia-containing gas mixture Γ by mixing the gas mixture with an aqueous liquid by which ammonia is at least partly absorbed, characterized in that the gas mixture and the aqueous liquid 14 are separately introduced into the inlet hood 15 of a tube bundle heat exchanger 16 and are mixed therein to obtain a twophase gas-liquid mixture 17', wherein subsequently the gas-liquid mixture is passed through the tubes of the tube bundle heat exchanger 16, wherein the gas-liquid mixture is cooled by a cooling medium guided on the shell· side, the gas-liquid mixture from the heat exchanger 16 subsequently is into a separator 18 for separating the gas and liquid phases, wherein a gas phase 19 depleted of ammonia and a liquid phase 12' enriched in ammonia are obtained and each discharged from the separator
    18 for the further use. _ \
  2. 2. The process according to claim 1 . characterized 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.
  3. 3. A process for separating ammonia from an ammonia-containing ' gas mixture by mixing the gas mixture with aqueous liquid by which the ammonia is at least partly absorbed, characterized in that the process is carried out in two steps, wherein the first step is effected according to claim ///-/1 or 2, then the gas phase 19 depleted of ammonia, which is obtained in the first step, is passed into an absorption column 2' and flows through the same from bottom to top, wherein fresh water 6' is introduced into the column, which flows through the absorption column 2' from top to bottom in counterflow to the gas phase, and wherein the gas 13' further depleted of ammonia is discharged from the column 12' for the further use, and wherein the water loaded with ammonia is discharged from the column 2' as aqueous liquid 14 and used in the first step, in that it is introduced into /// the inlet hood 15 of the tube bundle heat exchanger 16. - / .
    WO 2016/062410
    PCT/EP2015/025069 : x ;y) '
  4. 4. The process according to claim 3, characterized in that the absorption s· < ?<' ·';'column 2’ is equipped with two separate, superimposed mass transfer ; ' ·> ' devices 4’, 5' or structured packings, wherein the aqueous phase is ' ' + ';/· ; circulated over the tower packing 4' and for cooling guided over a heat
  5. 5 exchanger 10' located outside the column. ·'
    5. A plant 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 T and an aqueous liquid 14 and a discharge conduit
  6. 10 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', / Ϊ'' ' / x ' and for cooling the same, χ x. x · x 'XXx''x x <b) a separator 18 provided downstream of the plant section (a) for ; x'·' · χ· χ' separation into a liquid phase 12' enriched in ammonia and a gas phase 19 15 depleted of ammonia, χχ x < x x x (c) an absorption column 2' provided downstream of the plant section (b) ' χχ : χ with respect to the gas phase, containing a feed conduit for fresh water 6, x- χχΑ χ a discharge conduit for water loaded with ammonia as aqueous liquid 14, a χ xx χ 'χχχ^^ conduit for gas 13’ depleted of ammonia and at least one mass
    20 χ χx < transfer device 4‘, wherein a first part of the aqueous liquid 14 is delivered rover a heat exchanger 10’ by means of a delivery device 8', is cooled there • and subsequently again charged to the absorption column 2' above the χ χ x- mass transfer device 4', and wherein a second part of the aqueous liquid · 14 is recirculated to the plant section (a). · χχ χ x :
AU2015335275A 2014-10-22 2015-10-08 Process and plant for separating ammonia from a gas mixture Active AU2015335275B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102014115395.2A DE102014115395A1 (en) 2014-10-22 2014-10-22 Process and plant for the separation of ammonia from a gas mixture
DE102014115395.2 2014-10-22
PCT/EP2015/025069 WO2016062410A1 (en) 2014-10-22 2015-10-08 Process and plant for separating ammonia from a gas mixture

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AU2015335275A1 AU2015335275A1 (en) 2017-05-18
AU2015335275B2 true AU2015335275B2 (en) 2018-12-20

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AU (1) AU2015335275B2 (en)
DE (1) DE102014115395A1 (en)
EA (1) EA033528B1 (en)
WO (1) WO2016062410A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108889093B (en) * 2018-09-14 2024-03-19 深圳市奥图威尔科技有限公司 Waste gas treatment device for absorbing ammonia gas by using acetone

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3155722A (en) * 1960-01-29 1964-11-03 Chemical Construction Corp Recovery of residual ammonia and carbon dioxide in the synthesis of urea

Family Cites Families (6)

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Publication number Priority date Publication date Assignee Title
US3344585A (en) * 1967-05-12 1967-10-03 Eugene G Hollowell Method for recovering ammonia from gaseous mixture
DE10049227B4 (en) * 2000-09-28 2007-02-01 Bu Bioenergie & Umwelttechnik Ag Procedures for gas purification of process gas from gasification processes
RU2351385C1 (en) * 2007-10-29 2009-04-10 Общество с ограниченной ответственностью "Завод полимеров Кирово-Чепецкого химического комбината" (ООО "Завод полимеров КЧХК") Chlorine absorber
CN101439865A (en) * 2008-12-22 2009-05-27 江西稀有稀土金属钨业集团有限公司 Method for recycling ammine in ammonium paratungstate production
CN102087021B (en) * 2010-12-20 2014-04-09 华北电力大学 Integrated system for utilizing residual heat of boiler smoke and removing sulfur
CN203612972U (en) * 2013-10-23 2014-05-28 河南心连心化肥有限公司 Device for recycling ammonia from waste gas in ammonia synthetizing system

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3155722A (en) * 1960-01-29 1964-11-03 Chemical Construction Corp Recovery of residual ammonia and carbon dioxide in the synthesis of urea

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EA201790813A1 (en) 2017-08-31
CN105536433A (en) 2016-05-04
EA033528B1 (en) 2019-10-31
AU2015335275A1 (en) 2017-05-18
DE102014115395A1 (en) 2016-04-28
WO2016062410A1 (en) 2016-04-28
CN205412613U (en) 2016-08-03
CN105536433B (en) 2020-09-22

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