CN203593618U - Device for recycling hydrogen and ammonia in synthesis ammonia purge gas - Google Patents
Device for recycling hydrogen and ammonia in synthesis ammonia purge gas Download PDFInfo
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- CN203593618U CN203593618U CN201320844607.9U CN201320844607U CN203593618U CN 203593618 U CN203593618 U CN 203593618U CN 201320844607 U CN201320844607 U CN 201320844607U CN 203593618 U CN203593618 U CN 203593618U
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Abstract
The utility model discloses a device for recycling hydrogen and ammonia in synthesis ammonia purge gas. The device comprises a multi-channel-plate finned heat exchanger, a low-temperature gas-liquid separator, a gas-gas heat exchanger, a heater, a separating membrane and other main devices. Most ammonia in the synthesis ammonia purge gas is separated first through a throttling and expansion cooling technology, then an ammonia resisting membrane which can tolerate the fact that ammonia gas phase concentration is smaller than 6% (V/V) for a long time is used for recycling hydrogen and ammonia, safe and stable operation of a membrane separating process is guaranteed fundamentally, operation pressure of the synthesis ammonia purge gas is used, low-temperature gas is obtained by throttling and expansion cooling and is used as a cold source to separate ammonia in the purge gas in a condensation mode, and no extra power consumption exists. An obtained ammonia product is gas ammonia with the purity larger than 99% and is not weak ammonia water, ammonia recycling using is promoted, and at least 90% of hydrogen and at least 90% of ammonia are recycled in the mass.
Description
Technical field
The invention belongs to the technical field that synthetic ammonia relief gas reclaims, related in particular to a kind of from synthetic ammonia relief gas the device of recover hydrogen and ammonia.
Background technology
In production of synthetic ammonia, hydrogen and nitrogen are the raw materials of synthetic ammonia.Nitrogen is generally separated from air, and hydrogen generally obtains by conversion of natural gas or gasification, and hydrogen and nitrogen react under higher pressure and temperature and under catalyst action produces ammonia.Be subject to the restriction of chemical equilibrium, reactant can not transform completely, and unreacted nitrogen and hydrogen enter synthetic tower again and carries out ammonia synthesis reaction after recycle compressor mixes with supplementary virgin gas.Because synthetic ammonia feedstock nitrogen and hydrogen all contain a certain amount of inert component argon gas and methane, these inert components are constantly accumulation in working cycle, not only consume loop compression merit, also can make the useful volume of synthetic tower reduce, also can affect the normal reaction of synthetic ammonia, so synthetic tower mixed gas must discharge a part of gas, to control the concentration of inert component argon gas and methane in synthetic tower, this part discharge gas is called synthetic ammonia relief gas.Be about～300Nm of discharge tolerance
3/ ton ammonia, the classical group of this gas becomes: H250～70%(V/V), NH
31～8%(V/V), N
218～25%(V/V), remaining is methane and argon gas.
Mostly adopt at present membrane separation technique to fold into back and forth hydrogen and ammonia in ammonia relief gas.Because current mould material is to the non-constant of the tolerance of ammonia, so high pressure is speeded, venting must remove ammonia by pre-treatment before entering membrane separation apparatus, its method is generally and adopts isobaric washing in ammonia absorber, ammonia is removed, control the volume content of ammonia in gas phase below 0.02%, and then enter membrane separation apparatus reclaim speed venting in hydrogen, the hydrogen that the infiltration gas of film is enriching and recovering, turn back to synthesis system, the impermeable gas of film is mainly methane, nitrogen, argon gas and a small amount of hydrogen, uses as fuel.Aforesaid method is very strict to the operational requirement of ammonia absorber, can not occur ammonia concentration over-standard in gas phase, more will definitely avoid occurring the generation of entrainment and Concerning Flooding Phenomenon, otherwise can cause the expendable damage of downstream separation film.In actual application process, because ammonia absorber operation goes wrong, the example that causes separatory membrane to damage is very many.The weak ammonia simultaneously producing in water washing process, also needs further steam heating to purify and could arrive liquefied ammonia product, operating process complexity, and energy expenditure is high.
Summary of the invention
The object of the present invention is to provide a kind of technical process simple, energy consumption is low, easy to operate, operating safety, the method for hydrogen and ammonia in synthetic ammonia relief gas; It is a kind of for realizing described synthetic ammonia relief gas hydrogen and the device of ammonia that another object is to provide.The present invention adopts throttling to add swell refrigeration technology and first separates most ammonia in synthetic ammonia relief gas, then adopts and can withstand long term exposure ammonia phase concentration be less than 6%(V/V) the film of resistance to ammonia reclaim hydrogen and ammonia wherein.
2. in the synthetic ammonia relief gas described in, the device of hydrogen and ammonia comprises hyperchannel plate-fin heat exchanger, low temperature gas-liquid separator, gas-gas heat exchanger, well heater and separatory membrane, wherein:
3. the hyperchannel plate-fin heat exchanger described in is connected with low temperature gas-liquid separator; The outlet of low temperature gas-liquid separator liquefied ammonia is connected with throttling valve I, and is connected by hyperchannel plate-fin heat exchanger and gas ammonia recovery mouthful;
4. low temperature gas-liquid separator divides the outlet of ammonia tail gas by connecting multi-channel plate-fin heat exchanger, then is connected with gas-gas heat exchanger, well heater and separatory membrane successively;
5. the outlet of the per-meate side of separatory membrane, by gas-gas heat exchanger, is finally connected with synthetic compressor; The side outlet of holding back of separatory membrane is connected with watercooler, throttling valve II successively; By hyperchannel plate-fin heat exchanger, be connected with decompressor, fuel gas system successively again.
Of the present invention from synthetic ammonia relief gas the device of recover hydrogen and ammonia, its technical process mainly comprises throttling expansion process of refrigeration and membrane sepn process, wherein:
Described throttling expansion process of refrigeration: synthetic ammonia relief gas first enter into hyperchannel plate-fin heat exchanger cooling step by step after, enter low temperature gas-liquid separator and carry out gas-liquid separation; , after throttling valve I decompression, turn back to and be evaporated to gas ammonia after hyperchannel plate-fin heat exchanger and reclaim through the isolated liquefied ammonia of low temperature gas-liquid separator; Turn back to hyperchannel plate-fin heat exchanger through isolated point of low temperature gas-liquid separator top ammonia tail gas and reclaim after cold, then enter membrane sepn process; Wherein, by the tail gas after the separation liquefied ammonia out of low temperature gas-liquid separator top, be called a point ammonia tail gas.
Described membrane sepn process: through the gas of throttling expansion process of refrigeration processing, heat up through gas-gas heat exchanger, by well heater by behind gas heating to 45～90 ℃, pass through again separatory membrane processing, the gas of the per-meate side enrichment of separatory membrane, after gas-gas heat exchanger cooling, reclaims by synthetic compressor; The gas of holding back lateral enrichment of separatory membrane is down to after normal temperature through being arranged at the watercooler in its downstream, through throttling valve II, the pressure and temperature of gas is reduced; Enter into again expander refrigeration, this cryogenic gas is turned back to hyperchannel plate-fin heat exchanger and reclaim after cold, reclaim through fuel gas system.Wherein, 1. described well heater, its thermal source can be steam, deep fat, electricity or other high-temperature medium; Use well heater to improve gas and enter film temperature, guaranteed that gas departs from its dew-point temperature more than 10～30 ℃, to have prevented that liquid from condensing on film, causes the damage of film.Enter film gas temperature simultaneously and raise, can increase the permeation flux of film, reduce the investment of film system.2. divide ammonia tail gas to turn back to hyperchannel plate-fin heat exchanger, reclaim cold through re-heat.Then divide ammonia tail gas to pass through again gas-gas heat exchanger, with the seeping at high temperature gas heat exchange of membrane sepn process, improve the temperature of point ammonia tail gas, finally, by well heater, the temperature of gas is further raise, thereby guarantee that the temperature that enters membrane separation apparatus is at 45～90 ℃.
For technique scheme, in the preferred case, described separation membrane material is polyaramide.Conventional mould material, as polyimide, polysulfones all can not tolerate high ammonia concentration, so adopt the separatory membrane of polyaramide material in the present invention, this material can be less than 6%(V/V at ammonia phase concentration) condition under, life-time service.The characteristic of this mould material is that hydrogen and ammonia all preferentially permeate by film, in the per-meate side enrichment of film, then delivers to synthetic compressor entrance, turns back to ammonia synthesis system.Membrane process can be realized the recovery of ammonia more than more than 90% hydrogen and 80% in point ammonia tail gas.Separatory membrane hold back the membrane sepn tail gas that side is enrich methane, argon gas, nitrogen.
7. for technique scheme, in the preferred case, described throttling valve II is dropping valve, through throttling valve II, the pressure of gas is dropped to 1.0～4.0MPa.Described decompressor, it can drop to the temperature of gas-20～-70 ℃.
For technique scheme, in the preferred case, in described throttling expansion process of refrigeration, synthetic ammonia relief gas enters into hyperchannel plate-fin heat exchanger, and to be cooled to step by step temperature be-15～-50 ℃.
The present invention compared to existing technology tool has the following advantages:
1. the working pressure that utilizes synthetic ammonia relief gas itself, is freezed and is obtained cryogenic gas by throttling expansion, as low-temperature receiver, the ammonia condensing of speeding in venting is separated, and there is no extra power consumption.
2. traditional isobaric WATER-WASHING METHOD ammonia is reclaimed and compared, obtaining ammonolysis product is the gas ammonia that purity is greater than 99%, rather than weak ammonia, is conducive to the recycling of ammonia.
3. adopt and can withstand long term exposure ammonia phase concentration be less than 6%(V/V) the film of resistance to ammonia, from having guaranteed in essence safety, the steady running of membrane sepn process.
4. can guarantee the recovery of 90% above hydrogen and 90% above ammonia.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention;
Wherein, 1. hyperchannel plate-fin heat exchanger; 2. low temperature gas-liquid separator; 3. throttling valve I; 4. gas-gas heat exchanger; 5. well heater; 6. membrane separation apparatus; 7. watercooler; 8. throttling valve II; 9. decompressor.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail, can makes the present invention of those of ordinary skill in the art's comprehend, but not limit the present invention in any way.Pressure described in literary composition is gauge pressure.
Embodiment 1
In the synthetic ammonia relief gas of the recovery shown in Fig. 1 in the process flow diagram of the method for hydrogen and ammonia, the synthetic ammonia relief gas being discharged by synthesis system, its blowdown presssure is 14MPa, and temperature is-4 ℃, and tolerance is 20000Nm3/hr, composed as follows:
| Component | H 2 | N 2 | CH 4 | Ar | NH 3 |
| Content %(V) | 67.02 | 22.35 | 4.55 | 1.5 | 4.58 |
First this venting of speeding enters in hyperchannel plate-fin heat exchanger 1, and through stage-by-stage heat exchange, the temperature of off-gas drops to-21.50 ℃, and temperature drops to below the dew point of ammonia, and the phase of off-gas becomes gas-liquid two-phase.Gas-liquid mixture enters into low temperature gas-liquid separator 2, obtains liquid ammonia in the bottom of low temperature gas-liquid separator 2, and in condensation process, the rate of recovery of ammonia is 54%.Then liquefied ammonia is through throttling valve I 3, and decompression, to 0.25MPa, turns back to hyperchannel plate-fin heat exchanger 1, and cold is provided, and becomes gas ammonia product, and the purity of ammonia is at 99.5%(V), temperature is-14 ℃, turns back to existing ice maker intake header.
By point ammonia tail gas after the separation liquefied ammonia out of low temperature gas-liquid separator 2 tops, wherein the concentration of ammonia drops to 2.17%(V), turn back to hyperchannel plate-fin heat exchanger 1, reclaim cold through re-heat.Then divide ammonia tail gas to pass through again gas-gas heat exchanger 4, with the seeping at high temperature gas heat exchange of the membrane sepn process of membrane separation apparatus 6, the temperature of point ammonia tail gas is brought up to 18.5 ℃, finally by well heater 5, the temperature of gas is further elevated to 80 ℃, and 5 thermal source of well heater is low-pressure steam.Gas after intensification enters into membrane separation apparatus 6, and the separation membrane material using in membrane sepn process is polyaramide, after membrane sepn, obtains membrane permeate gas, and its pressure is 3.6MPa, and temperature is 80 ℃, and tolerance is 13469Nm3/hr, composed as follows:
| Component | H 2 | N 2 | CH 4 | Ar | NH 3 |
| Content %(V) | 92.32 | 3.97 | 0.53 | 0.53 | 2.65 |
Through the seeping at high temperature gas of membrane separation apparatus 6, after gas-gas heat exchanger 4 heat exchange, temperature drops to 30 ℃, delivers to synthetic compressor entrance.
Tail gas after membrane separation apparatus 6 separates, its pressure is 13.5MPa, and temperature is 80 ℃, and tolerance is 6035Nm3/hr, composed as follows:
| Component | H 2 | N 2 | CH 4 | Ar | NH 3 |
| Content %(V) | 16.04 | 65.19 | 13.89 | 3.80 | 1.08 |
In membrane separation apparatus 6 sepn processes, the rate of recovery of hydrogen is 92.7%, and the rate of recovery of ammonia is 39.1%.
The tail gas of membrane separation apparatus 6, drops to 40 ℃ by watercooler 7 by the temperature of the membrane sepn tail gas of membrane separation apparatus 6.Then the tail gas of membrane separation apparatus 6, through throttling valve II 8, from drop to～2.5MPa of high pressure, then enters into decompressor 9 by the pressure of gas, swell refrigeration, and the temperature of decompressor exit gas drops to-65 ℃.This cryogenic gas turns back to hyperchannel plate-fin heat exchanger 1, and cold is provided, and reduces the temperature of synthetic ammonia relief gas, and ammonia is wherein reclaimed in condensation.Be sent to fuel gas system from hyperchannel plate-fin heat exchanger membrane sepn tail gas as fuel gas.
Adopt throttling expansion refrigeration and membrane separation and integration technology, realized and from synthetic ammonia relief gas, reclaimed 92.7% hydrogen and 93.1% ammonia.
Embodiment 2
In the synthetic ammonia relief gas of the recovery shown in Fig. 1 in the process flow diagram of the method for hydrogen and ammonia, the synthetic ammonia relief gas being discharged by synthesis system, its blowdown presssure is 8.5MPa, and temperature is 8 ℃, and tolerance is 3500Nm3/hr, composed as follows:
| Component | H 2 | N 2 | CH 4 | Ar | NH 3 |
| Content %(V) | 62.2 | 20.43 | 7.58 | 3.34 | 6.45 |
First this venting of speeding enters in hyperchannel plate-fin heat exchanger 1, and through stage-by-stage heat exchange, the temperature of off-gas drops to-20 ℃, and temperature drops to below the dew point of ammonia, and the phase of off-gas becomes gas-liquid two-phase.Gas-liquid mixture enters into low temperature gas-liquid separator 2, obtains ammonia liquor in the bottom of low temperature gas-liquid separator 2, and in condensation process, the rate of recovery of ammonia is 48.3%.Then liquefied ammonia is through throttling valve I 3, and decompression, to 0.25MPa, turns back to hyperchannel plate-fin heat exchanger 1, and cold is provided, and becomes gas ammonia product, and the purity of ammonia is at 99.5%(V), temperature is-2 ℃, turns back to existing ice maker intake header.
By point ammonia tail gas after the separation liquefied ammonia out of low temperature gas-liquid separator 2 tops, wherein the concentration of ammonia drops to 3.44%(V), turn back to hyperchannel plate-fin heat exchanger 1, reclaim cold through re-heat.Then divide ammonia tail gas to pass through again gas-gas heat exchanger 4, with the seeping at high temperature gas heat exchange of the sepn process of membrane separation apparatus 6, the temperature of point ammonia tail gas is brought up to 24.9 ℃, finally by well heater 5, the temperature of gas is further elevated to 70 ℃, and 5 thermal source of well heater is low-pressure steam.Gas after intensification enters into membrane separation apparatus 6, and the separation membrane material using in the sepn process of membrane separation apparatus 6 is polyaramide, after membrane sepn, obtains membrane permeate gas, and its pressure is 2.5MPa, and temperature is 70 ℃, and tolerance is 2232Nm3/hr, composed as follows:
| Component | H 2 | N 2 | CH 4 | Ar | NH 3 |
| Content %(V) | 88.56 | 4.55 | 1.12 | 1.41 | 4.36 |
High temperature membrane permeate gas, after gas-gas heat exchanger 4 heat exchange, temperature drops to 35 ℃, delivers to synthetic compressor entrance.
Tail gas after membrane separation apparatus 6 separates, its pressure is 8.2MPa, and temperature is 70 ℃, and tolerance is 1157Nm3/hr, composed as follows:
| Component | H 2 | N 2 | CH 4 | Ar | NH 3 |
| Content %(V) | 17.24 | 52.98 | 20.74 | 7.37 | 1.67 |
In the membrane sepn process of membrane separation apparatus 6, the rate of recovery of hydrogen is 90.82%, and the rate of recovery of ammonia is 43.1%.
The separation tail gas of membrane separation apparatus 6, the temperature that membrane separation apparatus 6 is separated to tail gas by watercooler 7 drops to 38 ℃.Then the tail gas that membrane separation apparatus 6 separates, through throttling valve II 8, from drop to～2MPa of high pressure, then enters into decompressor 9 by the pressure of gas, swell refrigeration, and the temperature of decompressor 9 exit gass drops to-37 ℃.This cryogenic gas turns back to hyperchannel plate-fin heat exchanger 1, and cold is provided, and reduces the temperature of synthetic ammonia relief gas, and ammonia is wherein reclaimed in condensation.Be sent to fuel gas system from hyperchannel plate-fin heat exchanger 1 membrane sepn tail gas as fuel gas.
Adopt throttling expansion refrigeration and membrane separation and integration technology, realized and from synthetic ammonia relief gas, reclaimed 90.7% hydrogen and 91.4% ammonia.
Claims (3)
1. a device for recover hydrogen and ammonia from synthetic ammonia relief gas, is characterized in that: comprise hyperchannel plate-fin heat exchanger, low temperature gas-liquid separator, gas-gas heat exchanger, well heater and separatory membrane, wherein:
Described hyperchannel plate-fin heat exchanger is connected with low temperature gas-liquid separator; The outlet of low temperature gas-liquid separator liquefied ammonia is connected with throttling valve I, and is connected by hyperchannel plate-fin heat exchanger and gas ammonia recovery mouthful;
Low temperature gas-liquid separator divides the outlet of ammonia tail gas by connecting multi-channel plate-fin heat exchanger, then is connected with gas-gas heat exchanger, well heater and separatory membrane successively;
The per-meate side outlet of separatory membrane, by gas-gas heat exchanger, is finally connected with synthetic compressor; The side outlet of holding back of separatory membrane is connected with watercooler, throttling valve II successively; By hyperchannel plate-fin heat exchanger, be connected with decompressor, fuel gas system successively again.
According to claim 1 from synthetic ammonia relief gas the device of recover hydrogen and ammonia, it is characterized in that: described separation membrane material is polyaramide.
According to claim 1 from synthetic ammonia relief gas the device of recover hydrogen and ammonia, it is characterized in that: described throttling valve II is dropping valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320844607.9U CN203593618U (en) | 2013-12-18 | 2013-12-18 | Device for recycling hydrogen and ammonia in synthesis ammonia purge gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320844607.9U CN203593618U (en) | 2013-12-18 | 2013-12-18 | Device for recycling hydrogen and ammonia in synthesis ammonia purge gas |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190200A (en) * | 2014-08-15 | 2014-12-10 | 苏州市兴鲁空分设备科技发展有限公司 | Ammonia synthesis waste gas recycling device |
| CN108380009A (en) * | 2018-04-03 | 2018-08-10 | 中国科学院理化技术研究所 | Self-circulation device and method for removing white smoke |
| CN108946662A (en) * | 2017-05-18 | 2018-12-07 | 杭州福斯达深冷装备股份有限公司 | A kind of system recycling hydrogen from synthesis ammonia relief gas |
| CN113697772A (en) * | 2021-09-30 | 2021-11-26 | 杭州冰冷科技有限公司 | System and process method for recovering hydrogen and ammonia in synthetic ammonia purge gas |
-
2013
- 2013-12-18 CN CN201320844607.9U patent/CN203593618U/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190200A (en) * | 2014-08-15 | 2014-12-10 | 苏州市兴鲁空分设备科技发展有限公司 | Ammonia synthesis waste gas recycling device |
| CN104190200B (en) * | 2014-08-15 | 2016-05-11 | 苏州市兴鲁空分设备科技发展有限公司 | A kind of waste gas in synthesizing ammonia recycle device |
| CN108946662A (en) * | 2017-05-18 | 2018-12-07 | 杭州福斯达深冷装备股份有限公司 | A kind of system recycling hydrogen from synthesis ammonia relief gas |
| CN108380009A (en) * | 2018-04-03 | 2018-08-10 | 中国科学院理化技术研究所 | Self-circulation device and method for removing white smoke |
| CN108380009B (en) * | 2018-04-03 | 2024-09-20 | 中国科学院理化技术研究所 | Self-circulation device and method for flue gas whitening |
| CN113697772A (en) * | 2021-09-30 | 2021-11-26 | 杭州冰冷科技有限公司 | System and process method for recovering hydrogen and ammonia in synthetic ammonia purge gas |
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Granted publication date: 20140514 Termination date: 20171218 |