CN104913595B - It is a kind of to synthesize the method that ammonia relief gas carries hydrogen co-production of liquefied natural gas - Google Patents
It is a kind of to synthesize the method that ammonia relief gas carries hydrogen co-production of liquefied natural gas Download PDFInfo
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Abstract
The method of hydrogen co-production of liquefied natural gas is put forward the invention discloses a kind of synthesis ammonia relief gas, including washes ammonia, dehydration, liquefaction separation and PSA and puies forward four flows of hydrogen, separation can obtain LNG by liquefying, and carrying hydrogen by PSA obtains pure hydrogen.The present invention can reclaim in synthesis ammonia relief gas more than 90% methane and hydrogen, obtain the LNG (methane content >=98%) and pure hydrogen (hydrogen content >=99.99%) of high-purity；The characteristics of synthesis ammonia relief gas pressure is higher is made full use of, need not be pressurized into liquefaction separation unstripped gas, save the energy；Liquefaction separative element realizes the separation of hydrogen and methane using flash distillation mode, and more traditional rectifying mode is simple to operate, and need not provide external source, and energy consumption is low；The separative element that liquefies uses advanced mixed-refrigerant cycle technique, can be directed to the composition and ratio of different periodic off-gases adjustment of formula mix refrigerants, and more traditional nitrogen expansion refrigeration process energy consumption is low.
Description
Technical field
The present invention relates to a kind of comprehensive utilization technique for synthesizing ammonia relief gas, more particularly to a kind of synthesis ammonia relief gas is extracted
The method of hydrogen co-production liquefied natural gas.
Background technology
The energy resource structure feature of China is " rich coal, oil-poor, few gas ".The present situation of Natural Gas Resources in China shortage causes China
Natural gas applications are restricted.In recent years, due to factors such as energy security, climate change and environmental protection pressures, market for natural gas is entered
Enter the fast-developing phase, market for natural gas demand growth is rapid.
Synthesis ammonia is the basis of chemical industry, is also the pioneer of China's development of chemical industry, by the development of decades, I
State's ammonia synthesizing industry is greatly improved in terms of industry size, domestic self-supporting capability, technique device level.At present, I
Guohe's ammonification industry size has ranked first in the world, and total amount accounts for about 1/3rd of world's total amount.Due to experienced small nitrogen in history
Fertile, middle nitrogenous fertilizer, the evolution of big nitrogenous fertilizer, China's ammonia enterprise and nitrogenous fertilizer enterprises quantity are more, scattered distribution, industrial concentration
Low, overall technology level is not high.Synthesis gas is recycled in production of synthetic ammonia, and methane concentration can not be too high, therefore must
Must be by part containing the exhaust emissions (periodic off-gases) such as ammonia, hydrogen, methane, to control methane concentration, it is ensured that ammonia synthesis reaction it is normal
Carry out, its main component such as following table：
The synthesis ammonia relief gas typical case's composition of table 1
| Title | H2 | CH4 | N2 | NH3 | Ar |
| Constitute (mol%) | 50 | 22 | 20 | 3 | 5 |
The large and medium-sized fertilizer enterprises of China produce about 35,000,000 tons of ammonia of synthesis, gas and synthetic ammonia purge at least 3,300,000,000 Nm per year3.Mesh
It is preceding for synthesis ammonia relief gas, mainly there is two ways to be recycled：
One is, as fuel gas, to return to the burning of the equipment such as heating furnace.Due to containing many economic value addeds in periodic off-gases
Very high composition (such as hydrogen, methane), burns up as fuel, is very uneconomic in the lump.
Two be to use pressure-variable adsorption (PSA) or membrane separation technique purifying hydrogen of hydrogen, reclaims the hydrogen in synthesis ammonia relief gas, reaches
Sold to the volume increase of synthesis ammonia or as hydrogen product.Although realizing pairing in this way into the profit of hydrogen in ammonia relief gas
With, but methane, argon gas etc. can not be fully used.
The content of the invention
The purpose of the present invention be that provided to solve the above problems a kind of cryogenic separation plus pressure swing adsorption from
Synthesize ammonia relief gas in extract hydrogen simultaneously co-production of liquefied natural gas method, using the method, can from synthesis ammonia relief gas
The middle pure hydrogen and clean fuel liquefied natural gas for obtaining high added value, the problem of solving synthetic ammonia tailgas resource reclaim.
The present invention is achieved through the following technical solutions above-mentioned purpose：
It is a kind of to synthesize the method that ammonia relief gas carries hydrogen co-production of liquefied natural gas, comprise the following steps：
A1：Ammonia is washed, synthesis ammonia relief gas is introduced into Ammonic washing tower from bottom of towe, ammonia is carried out with the water counter current contacting from tower top
Absorb, the ammonia in unstripped gas is purified and below 200ppm purified gas is obtained；
A2：Dehydration, using two drying towers of adsorption tower and regenerator, by the purified gas obtained by step A1 from adsorption tower bottom
Portion enters, and by the adsorbent of molecular sieve adsorbing and removing moisture loaded in tower and obtains drying gas, and the regeneration source of the gas of regenerator is adopted
With the hydrogen rich gas of liquefaction separative element, regeneration gas delivers to PSA and carries hydrogen unit after regeneration；
A3：Liquefaction separation, the drying pneumatic transmission obtained in step A2 is entered in the main heat exchanger for the ice chest that liquefies heat exchange be cooled in advance-
120 DEG C, go out main heat exchanger, into rectifying tower bottom reboiler heat exchange cooling after return main heat exchanger continue cool down and liquefy
To -155 DEG C, go out main heat exchanger, flash tank is entered after being throttled by regulating valve, isolating hydrogen rich gas from flash tank returns to main heat exchanger
After re-heat to normal temperature, a part of hydrogen rich gas feeding PSA carries hydrogen unit, a part of then remove dewatering unit as source of the gas is regenerated, from sudden strain of a muscle
Enter rectifying column after the adjusted valve throttling of liquid of steaming pot outflow, rectifying column isolates methane, nitrogen and argon by cryogenic rectification
Gas, the nitrogen and argon gas of rectifying tower top outflow are diffused after returning to main heat exchanger re-heat to normal temperature, and the liquid of rectifying column bottom outflow is returned
Return main heat exchanger to cool and be cooled to after -160 DEG C, go out main heat exchanger, stored after throttling to LNG storage tank, that is, obtain liquefaction natural
Gas；
A4：PSA carries hydrogen, and the regeneration gas in the hydrogen rich gas and step A2 in step A3 enters from adsorption tower bottom of towe to be adsorbed
In tower, most impurity are removed under conditions of adsorbent selection absorption, the hydrogen that purity is more than 99.99% are obtained, from suction
Attached tower top is sent out after voltage stabilizing.
Further, the rich solution that ammonia is absorbed in step A1 is flowed out by the bottom of towe of Ammonic washing tower, and is passed through flash tank, by dodging
Removing fixed gas is steamed, and obtains the ammonifying again of high concentration to recycle, is returned to after the water after desorption is pressurized in Ammonic washing tower
Cyclic absorption.
Further, step A2 whole process is automatically performed by control system, and system pressure is by governor valve control.
Further, the liquefaction ice chest that drying gas resulting in step A2 enters in step A3 by dust filter unit.
Further, it is provided with to detect the dew point of dehydrating effect on the outlet process pipeline that gas is dried in step A2
Instrument, to ensure that the unstripped gas for entering liquefaction separative element meets technological requirement.
Further, the low-temperature receiver of main heat exchanger is provided by mixed-refrigerant cycle throttling expansion in step A3.
Further, it is that the liquefaction of natural gas is completed using the azeotrope refrigeration process with cryogenic rectification in step A3
And separation.
The beneficial effects of the present invention are：
The present invention can reclaim more than 90% methane and hydrogen and the LNG (first for obtaining high-purity in synthesis ammonia relief gas
Alkane content >=98%) and pure hydrogen (hydrogen content >=99.99%)；The characteristics of synthesis ammonia relief gas pressure is higher is made full use of, is entered
Entering liquefaction separation unstripped gas need not be pressurized, and save the energy；Liquefaction separative element realizes hydrogen and methane using flash distillation mode
Separation, more traditional rectifying mode is simple to operate, and need not provide external source, and energy consumption is low；Separative element liquefy using first
The mixed-refrigerant cycle technique entered, can be directed to the composition and ratio of different periodic off-gases adjustment of formula mix refrigerants, relatively pass
The nitrogen expansion refrigeration process energy consumption of system is low.
Embodiment
The invention will be further described below：
The present invention comprises the following steps：
A1：Ammonia is washed, synthesis ammonia relief gas is introduced into Ammonic washing tower from bottom of towe, ammonia is carried out with the water counter current contacting from tower top
Absorb, the ammonia in unstripped gas is purified and below 200ppm purified gas is obtained；
A2：Dehydration, using two drying towers of adsorption tower and regenerator, by the purified gas obtained by step A1 from adsorption tower bottom
Portion enters, and by the adsorbent of molecular sieve adsorbing and removing moisture loaded in tower and obtains drying gas, and the regeneration source of the gas of regenerator is adopted
With the hydrogen rich gas of liquefaction separative element, regeneration gas delivers to PSA and carries hydrogen unit after regeneration；
A3：Liquefaction separation, the drying pneumatic transmission obtained in step A2 is entered in the main heat exchanger for the ice chest that liquefies heat exchange be cooled in advance-
120 DEG C, go out main heat exchanger, into rectifying tower bottom reboiler heat exchange cooling after return main heat exchanger continue cool down and liquefy
To -155 DEG C, go out main heat exchanger, flash tank is entered after being throttled by regulating valve, isolating hydrogen rich gas from flash tank returns to main heat exchanger
After re-heat to normal temperature, a part of hydrogen rich gas feeding PSA carries hydrogen unit, a part of then remove dewatering unit as source of the gas is regenerated, from sudden strain of a muscle
Enter rectifying column after the adjusted valve throttling of liquid of steaming pot outflow, rectifying column isolates methane, nitrogen and argon by cryogenic rectification
Gas, the nitrogen and argon gas of rectifying tower top outflow are diffused after returning to main heat exchanger re-heat to normal temperature, and the liquid of rectifying column bottom outflow is returned
Return main heat exchanger to cool and be cooled to after -160 DEG C, go out main heat exchanger, stored after throttling to LNG storage tank, that is, obtain liquefaction natural
Gas；
A4：PSA carries hydrogen, and the regeneration gas in the hydrogen rich gas and step A2 in step A3 enters from adsorption tower bottom of towe to be adsorbed
In tower, most impurity are removed under conditions of adsorbent selection absorption, the hydrogen that purity is more than 99.99% are obtained, from suction
Attached tower top is sent out after voltage stabilizing.
The rich solution that ammonia is absorbed in step A1 is flowed out by the bottom of towe of Ammonic washing tower, and is passed through flash tank, by flashing removing not
Solidifying gas, and the ammonifying again of high concentration is obtained to recycle, return to cyclic absorption in Ammonic washing tower after the water after desorption is pressurized.
Step A2 whole process is automatically performed by control system, and system pressure is by governor valve control.
The liquefaction ice chest that drying gas obtained by step A2 enters in step A3 by dust filter unit.
In step A2 dry gas outlet process pipeline on be provided with to detect the dew point hygrometer of dehydrating effect, with ensure into
The unstripped gas for entering the separative element that liquefies meets technological requirement.
It is the liquefaction and separation that natural gas is completed using the azeotrope refrigeration process with cryogenic rectification in step A3, it is main
The low-temperature receiver of heat exchanger is provided by mixed-refrigerant cycle throttling expansion.Gas phase cryogen after being compressed through refrigerant compressor enters ice chest
Main heat exchanger heat exchange is cooled to -160 DEG C, goes out main heat exchanger, after adjusted valve throttling, as low-temperature receiver return main heat exchanger with it is cold
The heat exchange re-heats such as agent, dry gas.Liquid phase cryogen after being compressed through refrigerant compressor enter the heat exchange of ice chest main heat exchanger be cooled to-
60 DEG C, go out main heat exchanger, after adjusted valve throttling, return to main heat exchanger and cryogen as low-temperature receiver, dry the heat exchange re-heat such as gas.Through
The cryogen of main heat exchanger re-heat returns to refrigerant compressor entrance, completes kind of refrigeration cycle.Mix refrigerant nitrogen, methane, ethene, third
3-5 kind cryogens in alkane, 5 kinds of cryogens of isopentane are mixed by a certain percentage.The low-temperature receiver of rectifying tower top condenser is followed by nitrogen
Ring throttling expansion is provided.Nitrogen after being compressed through nitrogen compressor enters the heat exchange of ice chest main heat exchanger and is cooled to -160 DEG C, goes out master
Heat exchanger, after adjusted valve throttling, temperature is down to -185 DEG C, and entering rectifying tower top condenser as low-temperature receiver, there is provided condenser institute
The cold needed, returns again to return nitrogen compressor entrance after main heat exchanger re-heat to normal temperature, completes kind of refrigeration cycle.
Embodiment 1：
The unstripped gas of table 2 is constituted
| Title | H2 | CH4 | N2 | NH3 | Ar |
| Constitute (mol%) | 50 | 23 | 20 | 5 | 2 |
1) periodic off-gases component refers to table 2, and adjusted valve is depressurized to 4.0MPa；
2) periodic off-gases enter Ammonic washing tower, are purified by water absorption to ammonia≤200ppm；
3) purified gas enters drying tower, is less than -65 DEG C by the molecular sieve filling adsorbing and removing moisture in tower to dew point；
4) dry gas and enter liquefaction ice chest, by cryogenic separation, obtain the liquefied natural gas of methane molar concentration >=98%
And hydrogen rich gas；
5) liquefaction is using nitrogen, methane, ethene, propane, five component mix refrigerants of isopentane, each component molar fraction
For：Nitrogen 10%, methane 39.5%, ethene 20.5%, propane 16%, isopentane 14%；
6) hydrogen rich gas that liquefaction is separated enters PSA adsorption towers, passes through the selection adsorbing and removing overwhelming majority of adsorbent
Impurity, obtains the pure hydrogen of purity >=99.99%.
Embodiment 2：
The unstripped gas of table 3 is constituted
| Title | H2 | CH4 | N2 | NH3 | Ar |
| Constitute (mol%) | 45 | 30 | 20 | 3 | 2 |
1) periodic off-gases component refers to table 3, and adjusted valve is depressurized to 3.0MPa；
2) periodic off-gases enter Ammonic washing tower, are purified by water absorption to ammonia≤200ppm；
3) purified gas enters drying tower, is less than -65 DEG C by the molecular sieve filling adsorbing and removing moisture in tower to dew point；
4) dry gas and enter liquefaction ice chest, by cryogenic separation, obtain the liquefied natural gas of methane molar concentration >=98%
And hydrogen rich gas；
5) liquefaction is using nitrogen, methane, ethene, propane, five component mix refrigerants of isopentane, each component molar fraction
For：Nitrogen 10%, methane 37.5%, ethene 22%, propane 16%, isopentane 14.5%；
6) hydrogen rich gas that liquefaction is separated enters PSA adsorption towers, passes through the selection adsorbing and removing overwhelming majority of adsorbent
Impurity, obtains the pure hydrogen of purity >=99.99%.
Embodiment 3：
The unstripped gas of table 4 is constituted
| Title | H2 | CH4 | N2 | NH3 | Ar |
| Constitute (mol%) | 55 | 15 | 23 | 5 | 2 |
1) periodic off-gases component refers to table 4, and adjusted valve is depressurized to 3.0MPa；
2) periodic off-gases enter Ammonic washing tower, are purified by water absorption to ammonia≤200ppm；
3) purified gas enters drying tower, is less than -65 DEG C by the molecular sieve filling adsorbing and removing moisture in tower to dew point；
4) dry gas and enter liquefaction ice chest, by cryogenic separation, obtain the liquefied natural gas of methane molar concentration >=98%
And hydrogen rich gas；
5) liquefaction is using nitrogen, methane, ethene, propane, five component mix refrigerants of isopentane, each component molar fraction
For：Nitrogen 10%, methane 42%, ethene 21%, propane 15%, isopentane 13%；
6) hydrogen rich gas that liquefaction is separated enters PSA adsorption towers, passes through the selection adsorbing and removing overwhelming majority of adsorbent
Impurity, obtains the pure hydrogen of purity >=99.99%.
These are only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Any modifications, equivalent substitutions and improvements made within principle etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of synthesize the method that ammonia relief gas carries hydrogen co-production of liquefied natural gas, it is characterised in that comprises the following steps：
A1：Ammonia is washed, synthesis ammonia relief gas is introduced into Ammonic washing tower from bottom of towe, the suction of ammonia is carried out with the water counter current contacting from tower top
Receive, the ammonia in unstripped gas is purified and below 200ppm purified gas is obtained；
A2：Dehydration, using two drying towers of adsorption tower and regenerator, the purified gas obtained by step A1 is entered from absorption tower bottom
Enter, by the adsorbent of molecular sieve adsorbing and removing moisture loaded in tower and obtain drying gas, the regeneration source of the gas of regenerator uses liquid
Change the hydrogen rich gas of separative element, regeneration gas delivers to PSA and carries hydrogen unit after regeneration；
A3：Liquefaction separation, the drying pneumatic transmission obtained in step A2 is entered heat exchange in the main heat exchanger for the ice chest that liquefies and is cooled to -120 in advance
DEG C, go out main heat exchanger, into rectifying tower bottom reboiler heat exchange cooling after return main heat exchanger continue cool down and liquefy to-
155 DEG C, go out main heat exchanger, flash tank is entered after being throttled by regulating valve, isolate hydrogen rich gas return main heat exchanger from flash tank and answer
Heat is to after normal temperature, and a part of hydrogen rich gas feeding PSA carries hydrogen unit, a part of then remove dewatering unit as source of the gas is regenerated, from flash distillation
Enter rectifying column after the adjusted valve throttling of liquid of tank outflow, rectifying column isolates methane, nitrogen and argon gas by cryogenic rectification,
The nitrogen and argon gas of rectifying tower top outflow are diffused after returning to main heat exchanger re-heat to normal temperature, and the liquid of rectifying column bottom outflow returns to master
Heat exchanger, which cooled, to be cooled to after -160 DEG C, goes out main heat exchanger, is stored after throttling to LNG storage tank, that is, is obtained liquefied natural gas；
A4：PSA carries hydrogen, and the regeneration gas in the hydrogen rich gas and step A2 in step A3 enters adsorption tower from adsorption tower bottom of towe
In, most impurity are removed under conditions of adsorbent selection absorption, the hydrogen that purity is more than 99.99% are obtained, from absorption
Tower top is sent out after voltage stabilizing.
2. the method that synthesis ammonia relief gas according to claim 1 carries hydrogen co-production of liquefied natural gas, it is characterised in that：Step
The rich solution that ammonia is absorbed in A1 is flowed out by the bottom of towe of Ammonic washing tower, and is passed through flash tank, by flashing removing fixed gas, and obtains height
The ammonifying again of concentration returns to cyclic absorption in Ammonic washing tower to recycle after water after desorption is pressurized.
3. the method that synthesis ammonia relief gas according to claim 1 carries hydrogen co-production of liquefied natural gas, it is characterised in that：Step
A2 whole process is automatically performed by control system, and system pressure is by governor valve control.
4. the method that synthesis ammonia relief gas according to claim 1 carries hydrogen co-production of liquefied natural gas, it is characterised in that：Step
The liquefaction ice chest that drying gas obtained by A2 enters in step A3 by dust filter unit.
5. the method that synthesis ammonia relief gas according to claim 1 carries hydrogen co-production of liquefied natural gas, it is characterised in that：Step
It is provided with to detect the dew point hygrometer of dehydrating effect on the outlet process pipeline for drying gas in A2, it is single to ensure to enter liquefaction separation
The unstripped gas of member meets technological requirement.
6. the method that synthesis ammonia relief gas according to claim 1 carries hydrogen co-production of liquefied natural gas, it is characterised in that：Step
The low-temperature receiver of main heat exchanger is provided by mixed-refrigerant cycle throttling expansion in A3.
7. the method that synthesis ammonia relief gas according to claim 1 carries hydrogen co-production of liquefied natural gas, it is characterised in that：Step
It is the liquefaction and separation that natural gas is completed using the azeotrope refrigeration process with cryogenic rectification in A3.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN213811330U (en) * | 2020-09-16 | 2021-07-27 | 中国海洋石油集团有限公司 | Device for preparing liquid hydrogen by LNG |
| CN113446815B (en) * | 2021-09-01 | 2021-11-12 | 杭州制氧机集团股份有限公司 | Hydrogen liquefaction equipment adopting mixed refrigeration and using method thereof |
| CN114891546B (en) * | 2022-06-08 | 2022-12-09 | 佛燃能源集团股份有限公司 | System and method for preparing hydrogen and fuel-grade natural gas by using purge gas of synthetic ammonia |
| CN115851332B (en) * | 2022-12-26 | 2023-07-04 | 新疆凯龙清洁能源股份有限公司 | Method and system for preparing natural gas from tail gas of hydrogen extraction from synthetic ammonia purge gas membrane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3543529A (en) * | 1967-08-29 | 1970-12-01 | Helmut Knapp | Separation of ammonia synthesis off gas by engine expansion and separation |
| CN102827658A (en) * | 2012-08-30 | 2012-12-19 | 河南开元空分集团有限公司 | Method for preparing high-purity liquefied natural gas from ammonia synthesis tail 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 |
-
2015
- 2015-06-04 CN CN201510304545.6A patent/CN104913595B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3543529A (en) * | 1967-08-29 | 1970-12-01 | Helmut Knapp | Separation of ammonia synthesis off gas by engine expansion and separation |
| CN102827658A (en) * | 2012-08-30 | 2012-12-19 | 河南开元空分集团有限公司 | Method for preparing high-purity liquefied natural gas from ammonia synthesis tail 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 |
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