CN101590364A - Gas and synthetic ammonia purge and basin gas are carried out method and the device that hydrogen reclaims - Google Patents
Gas and synthetic ammonia purge and basin gas are carried out method and the device that hydrogen reclaims Download PDFInfo
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- CN101590364A CN101590364A CNA2009103040940A CN200910304094A CN101590364A CN 101590364 A CN101590364 A CN 101590364A CN A2009103040940 A CNA2009103040940 A CN A2009103040940A CN 200910304094 A CN200910304094 A CN 200910304094A CN 101590364 A CN101590364 A CN 101590364A
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Abstract
The invention discloses and a kind of gas and synthetic ammonia purge and basin gas are carried out method and the device that hydrogen reclaims, it washes ammonia treatment to off-gas and basin gas earlier, the pneumatic transmission accurate filter of washing behind the ammonia that discharges removes water smoke, enter membrane hydrogen separator after the preheater temperature adjustment, hydrogen in the off-gas utilizes overbottom pressure to return synthetic compressor in the per-meate side of membrane hydrogen separator, membrane hydrogen separator retentate side gas decompression back with wash ammonia after low-pressure tank gas mix, the mixed storage tank pneumatic transmission is gone into and is sent into the ice chest system after molecular sieve adsorber and dust filter unit are removed residual ammonia and water, and the gas of cooling box system is as hydrogen product and fuel gas.The present invention utilizes off-gas self high pressure to adopt membrane separation process recovery hydrogen wherein, film per-meate side hydrogen utilization overbottom pressure is returned synthetic compressor, the equipment complexity that has solved off-gas and basin gas independent recover hydrogen in the past and caused, make the maintenance cost height, the low shortcomings of the valuable gases rate of recovery such as hydrogen.
Description
Technical field
The present invention relates to a kind of method and device that gas and synthetic ammonia purge and basin gas are reclaimed, particularly a kind of method of gas and synthetic ammonia purge and basin gas being carried out the hydrogen recovery.
Background technology
Synthetic ammonia is mainstay of the national economy industry, and output occupies various chemical products first place.Also be major power consumer simultaneously, nearly in the world 10% the energy is used for synthetic ammonia.Along with increasingly sharpening of the energy, the dual crisis of environment, the energy-saving and emission-reduction of synthetic ammonia installation are imperative.The tail gas of synthetic ammonia mainly comprises off-gas (from the part circulating air of ammonia convertor extraction) and basin gas (gas that vacuum flashing goes out the anhydrous ammonia tank).The main component of synthetic ammonia tailgas is inert components such as ammonia, hydrogen nitrogen raw material and methane, argon gas, is the important measures that synthetic ammonia installation is energy-saving and cost-reducing and improve the business economic benefit from wherein extracting useful constituents such as hydrogen.
The main method that reclaims hydrogen in the synthetic ammonia tailgas at present has Deep Cooling Method, membrane separation process and pressure swing adsorption method etc., three kinds of methods cut both ways: cryogenic technology adopts the pressure of off-gas itself to carry out the swell refrigeration cooling, makes other component liquefactions to reach the purpose that hydrogen is separated.Density of hydrogen and yield all can reach 90%, and treating capacity is big, but investment is big, the energy consumption height; Pressure swing adsorption method is lower for ingredient requirement, and the density of hydrogen of recovery can reach 99%, and equipment is simple, advantage of low energy consumption, but has the weak point of the hydrogen rate of recovery low (about 60%), the easy efflorescence of adsorbent; The obvious advantage of membrane separation process is no rotating machinery, utilizes the high pressure of gas and synthetic ammonia purge, implements meritorious step-down, and product hydrogen can utilize overbottom pressure to send synthesis system back to, therefore need not power consumption.Density of hydrogen, the rate of recovery are all more than 90%, but film separates having relatively high expectations to unstripped gas.
In the hydrogen of synthetic ammonia tailgas reclaimed, being used alone or in combination still of said method came with some shortcomings.Be embodied in: because the pressure of off-gas and basin gas differs bigger, at present, synthesis ammonia plant or the hydrogen in the recovering discharging gas only, basin gas reclaim only to be made fuel behind the ammonia and uses, thereby reduces its value greatly; Perhaps off-gas and basin gas are separated and carry out the hydrogen recovery, increased considerably equipment investment like this, the overall recovery of these methods recover hydrogen from synthetic ammonia tailgas is also relatively low simultaneously.
Summary of the invention
The objective of the invention is to, what provide that a kind of equipment investment is few, the hydrogen overall recovery is high carries out method and the device that hydrogen reclaims to gas and synthetic ammonia purge and basin gas, can overcome the deficiencies in the prior art.
Technical scheme of the present invention: it washes ammonia treatment respectively to off-gas and basin gas earlier, wash discharging behind the ammonia and enter membrane hydrogen separator after the pneumatic transmission accurate filter removes water smoke, preheater temperature adjustment, hydrogen in the off-gas utilizes overbottom pressure to return synthetic compressor in the per-meate side of membrane hydrogen separator, membrane hydrogen separator retentate side gas decompression back with wash ammonia after low-pressure tank gas mix, the mixed storage tank pneumatic transmission is gone into and is sent into the ice chest system after molecular sieve adsorber and dust filter unit are removed residual ammonia and water, and the gas of cooling box system is as hydrogen product and fuel gas.
Off-gas and basin gas adopt off-gas Ammonic washing tower and basin gas Ammonic washing tower to wash ammonia respectively.
The temperature of advancing membrane hydrogen separator is adjusted to 40～60 ℃ by preheater.
The temperature of ice chest system is subzero 180～190 ℃, and most of methane, argon gas, nitrogen and a part of hydrogen in the mixed storage tank gas are liquefied, and produces gas-liquid two-phase in the ice chest, and Ye Hua hydrogen does not separate through hydrogen separator.
The quantity of molecular sieve adsorber is two, and two molecular sieve adsorbers are used alternatingly, when residual ammonia and water are by a molecular sieve adsorber absorption in the gas, and another molecular sieve adsorber thermal regeneration.
The ice chest system relies on gas throttling to produce cold, and is provided with plate-fin heat exchanger in the ice chest system, mixed storage tank gas in plate-fin heat exchanger with throttling after the heat exchange of low temperature product.
The gas of hydrogen separator outlet, liquid two-phase produce cold through decompression respectively, carry out reverse heat-exchange with the gaseous mixture that enters the ice chest system after, gas phase is as hydrogen product, the liquid phase gas that acts as a fuel leaves ice chest.
Gas and synthetic ammonia purge and basin gas are carried out device that hydrogen reclaims to be comprised and discharges tracheae and basin tracheae, discharging tracheae is connected with basin gas Ammonic washing tower with the off-gas Ammonic washing tower respectively with the basin tracheae, be connected with different vapour liquid separator by pipeline respectively in the upper end of off-gas Ammonic washing tower and basin gas Ammonic washing tower, with vapour liquid separator that the off-gas Ammonic washing tower is connected on be connected with accurate filter by pipeline, accurate filter is connected with preheater by pipeline, preheater is connected with membrane hydrogen separator, on membrane hydrogen separator, be provided with infiltration side pipe and retentate side pipe, the infiltration side pipe is connected with synthesic gas compressor, the retentate side pipe was connected on the vapour liquid separator that basin gas Ammonic washing tower connects and the pipeline that molecular sieve is connected, molecular sieve is connected with dust filter unit by pipeline, dust filter unit is connected with the ice chest system, be provided with plate-fin heat exchanger in the ice chest system, the ice chest system is connected with hydrogen separator by pipeline.
On the infiltration side pipe, be connected with pressure-reducing valve.
Be connected with pressure-reducing valve respectively on the gas liquid outlet pipe of hydrogen separator, the gas liquid outlet pipe of hydrogen separator is connected in the ice chest system.
Compared with the prior art, the present invention washes ammonia treatment to off-gas and basin gas earlier, wash discharging behind the ammonia and enter membrane hydrogen separator after the pneumatic transmission accurate filter removes water smoke, preheater temperature adjustment, hydrogen in the off-gas returns synthetic compressor in the per-meate side of membrane hydrogen separator with overbottom pressure, membrane hydrogen separator retentate side gas decompression back with wash ammonia after low-pressure tank gas mix, the mixed storage tank pneumatic transmission is gone into and is sent into the ice chest system after molecular sieve adsorber and dust filter unit are removed residual ammonia and water, and the gas of cooling box system is as hydrogen product and fuel gas.So just can utilize off-gas self high pressure to adopt membrane separation process recovery hydrogen wherein, film per-meate side hydrogen utilization overbottom pressure is returned synthetic compressor, basin gas after oozing residual air decompression back and washing ammonia mixes, send into ice chest purification hydrogen wherein, the equipment complexity that has solved off-gas and basin gas independent recover hydrogen in the past and caused, make the maintenance cost height, the low shortcomings of the valuable gases rate of recovery such as hydrogen.Be particularly suitable for self having the synthesis ammonia plant of cryogenic separation unit.Off-gas and basin gas adopt off-gas Ammonic washing tower and basin gas Ammonic washing tower to wash ammonia respectively, like this gas with spray the soft water that gets off by cat head and carry out reverse the contact, most ammonia can be water-washed away; The temperature of advancing membrane hydrogen separator is adjusted to 40～60 ℃ by preheater, can guarantee the normal operation of membrane hydrogen separator like this.
The applicant has carried out substantive test to the present invention simultaneously, and two groups of test datas of existing arbitrarily extraction are calculated the rate of recovery of hydrogen of the present invention:
Off-gas in example one, the production and basin destiny are according to as follows:
Be not more than 100PPM and calculate to wash behind the ammonia in the gas ammonia content, ammonia concn is about 31% and 24% respectively at the bottom of off-gas, the basin air purge ammonia Tata.
The membrane hydrogen separator gas data is as follows:
Ice chest system gas data are as follows:
Hydrogen overall recovery of the present invention after testing can reach 99.5%.
Example two: off-gas in the production and basin destiny are according to as follows:
Be not more than 100PPM and calculate to wash behind the ammonia in the gas ammonia content, ammonia concn is respectively about 22% and 14% at the bottom of off-gas, the basin air purge ammonia Tata.
The membrane hydrogen separator gas data:
Ice chest system gas data:
Hydrogen overall recovery of the present invention after testing can reach 98.89%.
Can find out obviously that from above two groups of test datas hydrogen overall recovery of the present invention can produce significant impact far above the rate of recovery of hydrogen in the existing recovery synthetic ammonia tailgas to energy-saving and cost-reducing and raising business economic benefit, has good practical and popularizing value.
Description of drawings
Fig. 1 is a structural representation of the present invention.
The specific embodiment
Embodiment 1: as shown in Figure 1, adopt off-gas Ammonic washing tower 1 and basin gas Ammonic washing tower 6 respectively off-gas and basin gas to be washed ammonia treatment, remove ammonia wherein, off-gas and basin gas with spray the soft water that gets off by cat head and carry out reverse the contact, overwhelming majority ammonia is water-washed away, and the product of Ammonic washing tower bottom is the ammonia spirit of the about 20-30% of concentration; Cat head deamination gas removes the aqueous water of carrying secretly through vapour liquid separator 2, ammonia content＜200PPM in the gained gas.Wash that hydrogen content is about 60% in the off-gas behind the ammonia; The off-gas of washing behind the ammonia is removed water smoke through accurate filter 3, enters membrane hydrogen separator 5 after preheater 4 adjusts the temperature to 40-60 ℃.The synthesis pressure of synthetic ammonia generally about 13-30MPa, if enter membrane hydrogen separator 5 recover hydrogen, need be decompressed to about 12MPa usually.Hydrogen molecule in off-gas penetrated preferably in polymeric film material obtains hydrogen in per-meate side; Nitrogen, methane and argon gas etc. then major part are trapped in the retentate side of membrane hydrogen separator 5 high pressure, and infiltration gas utilizes overbottom pressure directly to return synthesic gas compressor as raw material along permeating side pipe; Ooze residual air by the retentate side pipe through behind the pressure-reducing valve with wash ammonia after the basin atmospheric pressure equate, and by the retentate side pipe with wash ammonia after low-pressure tank gas mix, after removing residual ammonia and water, process molecular sieve 7 and dust filter unit 8 send into ice chest system 9, cold in the ice chest system 9 is produced by throttling, and the gas of cooling box system 9 is respectively as hydrogen product and fuel gas.Molecular sieve adsorber 7 two molecular sieve adsorbers for being used alternatingly, when residual ammonia and water are by 7 absorption of a molecular sieve adsorber in the gas, another molecular sieve adsorber 7 thermal regenerations, ammonia and the water of separating sucking-off are sent to the off-gas system.In ice chest system 9, be provided with plate-fin heat exchanger, the mixed storage tank gas that enters ice chest system 9 in plate-fin heat exchanger with throttling after the heat exchange of low temperature product, temperature is reduced to subzero approximately 180～190 ℃, make wherein most of methane, argon gas, nitrogen and a part of liquefaction of hydrogen, and separate through hydrogen separator 10.Gas, the liquid two-phase of hydrogen separator 10 outlet produce cold through decompression respectively, and after mixing gas and carry out reverse heat-exchange with the mixed storage tank that enters ice chest system 9 respectively in plate-fin heat exchanger, gas phase is left ice chest system 9 as hydrogen product, the liquid phase gas that acts as a fuel.
Claims (10)
1. one kind is carried out the method that hydrogen reclaims to gas and synthetic ammonia purge and basin gas, it is characterized in that: it washes ammonia treatment to off-gas and basin gas earlier, the pneumatic transmission accurate filter of washing behind the ammonia that discharges removes water smoke, enter membrane hydrogen separator after the preheater temperature adjustment, hydrogen in the off-gas utilizes overbottom pressure to return synthetic compressor in the per-meate side of membrane hydrogen separator, the gas of membrane hydrogen separator retentate side decompression back with wash ammonia after low-pressure tank gas mix, the mixed storage tank pneumatic transmission is gone into and is sent into the ice chest system after molecular sieve adsorber and dust filter unit are removed residual ammonia and water, and the gas of cooling box system is as hydrogen product and fuel gas.
2. according to claim 1 gas and synthetic ammonia purge and basin gas are carried out the method that hydrogen reclaims, it is characterized in that: off-gas and basin gas adopt off-gas Ammonic washing tower and basin gas Ammonic washing tower to wash ammonia respectively.
3. according to claim 1 gas and synthetic ammonia purge and basin gas are carried out the method that hydrogen reclaims, it is characterized in that: the temperature of advancing membrane hydrogen separator is adjusted to 40～60 ℃ by preheater.
4. according to claim 1 gas and synthetic ammonia purge and basin gas are carried out the method that hydrogen reclaims, it is characterized in that: the temperature of ice chest system is subzero 180～190 ℃, most of methane, argon gas, nitrogen and a part of hydrogen in the mixed storage tank gas are liquefied, produce gas-liquid two-phase in the ice chest, Ye Hua hydrogen does not separate through hydrogen separator.
5. described gas and synthetic ammonia purge and basin gas are carried out the method that hydrogen reclaims according to claim 1 or 4, it is characterized in that: the quantity of molecular sieve adsorber is two, two molecular sieve adsorbers are used alternatingly, when residual ammonia and water were by a molecular sieve adsorber absorption in the gas, another molecular sieve adsorber was heated regeneration.
6. according to claim 4 gas and synthetic ammonia purge and basin gas are carried out the method that hydrogen reclaims, it is characterized in that: the ice chest system relies on gas throttling to produce cold, and in the ice chest system, be provided with plate-fin heat exchanger, mixed storage tank gas in plate-fin heat exchanger with throttling after the heat exchange of low temperature product.
7. according to claim 4 gas and synthetic ammonia purge and basin gas are carried out the method that hydrogen reclaims, it is characterized in that: gas, the liquid two-phase of hydrogen separator outlet produce cold through decompression respectively, after carrying out reverse heat-exchange with the gaseous mixture that enters the ice chest system, gas phase is left ice chest as hydrogen product, the liquid phase gas that acts as a fuel.
8. one kind is carried out the device that hydrogen reclaims to gas and synthetic ammonia purge and basin gas, it comprises and discharges tracheae and basin tracheae, it is characterized in that: discharge tracheae and be connected with basin gas Ammonic washing tower (6) with off-gas Ammonic washing tower (1) respectively with the basin tracheae, be connected with different vapour liquid separator (2) by pipeline respectively in the upper end of off-gas Ammonic washing tower (1) and basin gas Ammonic washing tower (6), upward be connected with accurate filter (3) at the vapour liquid separator (2) that is connected with off-gas Ammonic washing tower (1) by pipeline, accurate filter (3) is connected with preheater (4) by pipeline, preheater (4) is connected with membrane hydrogen separator (5), on membrane hydrogen separator (5), be provided with infiltration side pipe and retentate side pipe, the infiltration side pipe is connected with synthesic gas compressor, the retentate side pipe was connected on the vapour liquid separator (2) that basin gas Ammonic washing tower (6) connects and the pipeline that molecular sieve adsorber (7) is connected, molecular sieve adsorber (7) is connected with dust filter unit (8) by pipeline, dust filter unit (8) is connected with ice chest system (9), be provided with plate-fin heat exchanger in ice chest system (9), ice chest system (9) is connected with hydrogen separator (10) by pipeline.
9. according to claim 8 gas and synthetic ammonia purge and basin gas are carried out the device that hydrogen reclaims, it is characterized in that: on the infiltration side pipe, be connected with pressure-reducing valve.
10. according to claim 8 gas and synthetic ammonia purge and basin gas are carried out the device that hydrogen reclaims, it is characterized in that: be connected with pressure-reducing valve respectively on the gas liquid outlet pipe of hydrogen separator (10), the gas liquid outlet pipe of hydrogen separator (10) is connected in the ice chest system (9).
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| CN2009103040940A CN101590364B (en) | 2009-07-07 | 2009-07-07 | Method and device for recovering hydrogen on purge gas in synthetic ammonia and gas stored in tank |
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| CN2009103040940A CN101590364B (en) | 2009-07-07 | 2009-07-07 | Method and device for recovering hydrogen on purge gas in synthetic ammonia and gas stored in tank |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530990A (en) * | 2011-12-22 | 2012-07-04 | 天邦膜技术国家工程研究中心有限责任公司 | Method for recovering hydrogen and ammonia from synthetic ammonia purge gas by membrane separation-rectification integrated technology and device |
| CN102583439A (en) * | 2012-02-08 | 2012-07-18 | 浠水县福瑞德化工有限责任公司 | Available gas recovery method in ammonia synthesis process |
| CN103663367A (en) * | 2013-12-18 | 2014-03-26 | 大连欧科膜技术工程有限公司 | Method for recovering hydrogen and ammonia in synthetic ammonia exhausted gas |
| CN103925773A (en) * | 2013-11-05 | 2014-07-16 | 北京蓝图工程设计有限公司 | Method for using synthetic ammonia tail gas to prepare liquefied natural gas and nitrogen and hydrogen |
| CN105565270A (en) * | 2016-02-04 | 2016-05-11 | 河南心连心化肥有限公司 | Device and process for recovering hydrogen in synthetic ammonia purge gas |
| CN112279216A (en) * | 2020-11-16 | 2021-01-29 | 河南骏化发展股份有限公司 | Device and process for preparing hydrogen for fuel cell by using synthetic ammonia purge gas |
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| US4687498A (en) * | 1986-02-24 | 1987-08-18 | The Boc Group, Inc. | Argon recovery from hydrogen depleted ammonia plant purge gas utilizing a combination of cryogenic and non-cryogenic separating means |
| FR2767529B1 (en) * | 1997-08-25 | 1999-10-08 | Inst Francais Du Petrole | METHOD AND UNIT FOR HYDROPROCESSING AN OIL LOAD COMPRISING CRACKING AMMONIA AND RECYCLING HYDROGEN IN THE UNIT |
| AU2752300A (en) * | 1999-02-03 | 2000-08-25 | Texaco Development Corporation | Utilizing purge gas from ammonia synthesis |
| JP2001226116A (en) * | 2000-02-16 | 2001-08-21 | Hitachi Zosen Corp | Method for manufacturing aqueous ammonia solution |
| CN1850586B (en) * | 2006-05-25 | 2010-09-08 | 山东晋煤明水化工集团有限公司 | Process and equipment for extracting hydrogen from air discharged from synthetic ammonia tank |
| CN200951883Y (en) * | 2006-07-05 | 2007-09-26 | 北京科瑞赛斯气体液化技术有限公司 | Recovering apparatus of synthesizing ammonia relax dischanging gaseous ammonia |
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2009
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530990A (en) * | 2011-12-22 | 2012-07-04 | 天邦膜技术国家工程研究中心有限责任公司 | Method for recovering hydrogen and ammonia from synthetic ammonia purge gas by membrane separation-rectification integrated technology and device |
| CN102583439A (en) * | 2012-02-08 | 2012-07-18 | 浠水县福瑞德化工有限责任公司 | Available gas recovery method in ammonia synthesis process |
| CN102583439B (en) * | 2012-02-08 | 2013-07-24 | 浠水县福瑞德化工有限责任公司 | Available gas recovery method in ammonia synthesis process |
| CN103925773A (en) * | 2013-11-05 | 2014-07-16 | 北京蓝图工程设计有限公司 | Method for using synthetic ammonia tail gas to prepare liquefied natural gas and nitrogen and hydrogen |
| CN103925773B (en) * | 2013-11-05 | 2016-08-17 | 北京蓝图工程设计有限公司 | A kind of synthetic ammonia tailgas prepares liquefied natural gas and the method for nitrogen hydrogen |
| CN103663367A (en) * | 2013-12-18 | 2014-03-26 | 大连欧科膜技术工程有限公司 | Method for recovering hydrogen and ammonia in synthetic ammonia exhausted gas |
| CN103663367B (en) * | 2013-12-18 | 2015-04-08 | 大连欧科膜技术工程有限公司 | Method for recovering hydrogen and ammonia in synthetic ammonia exhausted gas |
| CN105565270A (en) * | 2016-02-04 | 2016-05-11 | 河南心连心化肥有限公司 | Device and process for recovering hydrogen in synthetic ammonia purge gas |
| CN112279216A (en) * | 2020-11-16 | 2021-01-29 | 河南骏化发展股份有限公司 | Device and process for preparing hydrogen for fuel cell by using synthetic ammonia purge gas |
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