CN103123203B - Method of preparing pure nitrogen by using exhaust gas with nitrogen to carry out once-more cryogenic distillation - Google Patents
Method of preparing pure nitrogen by using exhaust gas with nitrogen to carry out once-more cryogenic distillation Download PDFInfo
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- CN103123203B CN103123203B CN201310056697.XA CN201310056697A CN103123203B CN 103123203 B CN103123203 B CN 103123203B CN 201310056697 A CN201310056697 A CN 201310056697A CN 103123203 B CN103123203 B CN 103123203B
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 270
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 121
- 239000007789 gas Substances 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000004821 distillation Methods 0.000 title abstract 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000001301 oxygen Substances 0.000 claims abstract description 108
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 108
- 239000007788 liquid Substances 0.000 claims abstract description 94
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 8
- 230000000630 rising effect Effects 0.000 claims abstract description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 64
- 239000002912 waste gas Substances 0.000 claims description 62
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 28
- 230000006835 compression Effects 0.000 claims description 17
- 238000007906 compression Methods 0.000 claims description 17
- 238000000746 purification Methods 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000004215 Carbon black (E152) Substances 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 6
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 6
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- 230000001186 cumulative effect Effects 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000004078 cryogenic material Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000003303 reheating Methods 0.000 abstract 2
- 238000000605 extraction Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 7
- 239000000284 extract Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011027 product recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000003584 silencer Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
- F25J3/04321—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of oxygen
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
- F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/04—Mixing or blending of fluids with the feed stream
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention discloses a method of preparing pure nitrogen by using exhaust gas with nitrogen to carry out two-stage cryogenic distillation. Purified raw material gas entering a fractionating tower system passes through a main heat exchanger to get cooled, and then enters a lower rectifying tower to get rectified. Pure nitrogen is obtained on the top portion of the lower rectifying tower, and oxygen-enriched liquid air is obtained on the bottom portion of the lower rectifying tower, a part of the obtained pure nitrogen is collected as product after reheating, and a part of the obtained pure nitrogen is used to supply reflux and product liquid nitrogen for the lower rectifying tower after cooling. The bottom portion oxygen-enriched liquid air enters an upper rectifying tower to get rectified. Exhaust gas with nitrogen is obtained on the top portion of the upper rectifying tower, and the oxygen-enriched liquid air is obtained on the bottom portion of the upper rectifying tower. The exhaust gas enters an air compressor after reheating, and is used as raw material gas after being mixed with air from the air compressor. A part of the oxygen-enriched liquid air of the upper rectifying tower is safely discharged, and the rest of the oxygen-enriched liquid air is heated to evaporate, a part of the evaporated oxygen-enriched liquid air is extracted from the bottom portion of the upper rectifying tower and used as expanding gas, and a part of the evaporated oxygen-enriched liquid air is used as rising gas of the upper rectifying tower. By using the method to prepare pure nitrogen, the extraction ratio of nitrogen product can be improved, running energy consumption of a device can be reduced, and the method of preparing the pure nitrogen by using the exhaust gas with the nitrogen to carry out the two-stage cryogenic distillation has significant economic benefit and social benefit.
Description
Technical field
The present invention relates to a kind of method producing nitrogen, belong to cryogenic air separation field, especially relate to a kind of method utilizing nitrogenous waste gas to carry out cryogenic rectification purity nitrogen again.
Background technology
Along with socioeconomic development, in recent years, the air separation plant application producing nitrogen is constantly expanded, and the requirement higher to energy-saving and cost-reducing proposition.How to improve the recovery rate of product, reduce the operation energy consumption of equipment, become the research direction of cryogenic rectification method nitrogen producing craft.The flow process pattern of Conventional cryogenic rectifying legal system nitrogen has single-stage rectifying waste expansion flow process and single-stage rectifying air expansion flow process two kinds.Wherein, single-stage rectifying waste expansion product nitrogen gas pressure is at 0.45 ~ 0.9MPa, and directly give user after product nitrogen gas cooling box and use, nitrogen product recovery rate is generally 45% ~ 58%; Single-stage rectifying air expanded product nitrogen pressure is at 0.175 ~ 1.35MPa, and nitrogen product recovery rate is probably 58% ~ 64%.
Summary of the invention
The technical problem to be solved in the present invention is: the defects such as the recovery rate existed for existing single-stage rectifying waste expansion flow process and single-stage rectifying air expansion flow process two kinds of techniques is low, energy consumption is high, the invention provides a kind of utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen.Technical solution of the present invention take to reclaim there is certain pressure the nitrogenous waste gas that backflows to air compressor three grades of entrances, mix with the raw air through air compressor two-stage compression recompress, precooling, purification, finally liquefy in fractionating column system, rectifying produce nitrogen.Adopting technical solution of the present invention to produce purity nitrogen, can improve the recovery rate of nitrogen product, reduce the operation energy consumption of device, is the technique that a kind of novel stream backed expansion produces nitrogen.
In order to solve the problem, the technical solution used in the present invention is:
The invention provides a kind of utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, said method comprising the steps of:
A, with 1000 purity nitrogen equipment for benchmark, produce purity nitrogen using air as the first unstripped gas, from the nitrogenous waste gas of fractionating column system as the second unstripped gas, first by the first unstripped gas air with 2000 ~ 2200Nm
3the intake of/h sends into air cleaner, dust in air cleaner removing air and impurity, then enter air compressor and be compressed into 0.19 ~ 0.46 MPa(a), the pressure simultaneously from fractionating column system is 0.317 ~ 0.46 MPa(a) the nitrogenous waste gas of the second unstripped gas with 300 ~ 550 Nm
3the intake of/h enters air compressor and the first unstripped gas carries out being mixed to get the 3rd unstripped gas, 3rd unstripped gas enters air compressor from air compressor next stage entrance again and compresses, compression eventually last pressure is 0.75 ~ 1.1 MPa(a), the 3rd unstripped gas after compression cools the temperature to 5 ~ 8 DEG C through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and purifies, the 3rd unstripped gas after being purified;
The 3rd unstripped gas after b, step a purification enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as upflowing vapor, is separated, obtains 2300 ~ 2780 Nm at lower rectifying column top through rectifying
3the pure nitrogen gas of/h, in gained pure nitrogen gas 35 ~ 45% DEG C to collect as product nitrogen gas through main heat exchanger re-heat to 5 ~ 7; Residual income pure nitrogen gas is cooled to liquid nitrogen in condenser/evaporator, the gained liquid nitrogen of wherein≤4% is discharged as nitrogen products and is collected, remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying is separated, obtain oxygen-enriched liquid air 1300 ~ 1700 Nm containing oxygen 32 ~ 35% in the bottom of lower rectifying column
3/ h, gained oxygen-enriched liquid air sends into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air sending into upper rectifying column in c, step b is separated through rectifying, obtains waste gas 300 ~ 550 Nm of nitrogenous volumn concentration 81 ~ 83% at upper rectifying column top
3/ h, the nitrogenous waste gas of gained sends into the inter-stage entrance of air compressor in step a as the second unstripped gas; The bottom of upper rectifying column obtains oxygen enriched liquid 1100 ~ 1560 Nm containing oxygen 62 ~ 67%
3/ h, the oxygen enriched liquid wherein accounting for gained oxygen enrichment volume 0.5 ~ 0.8% directly discharges fractionating column system, as safety dumping, residue oxygen enriched liquid by the nitrogen heating and gasifying that lower rectifying column top obtains, obtains the oxygen-enriched liquid air vapor containing oxygen 38 ~ 41% in condenser/evaporator; The oxygen-enriched liquid air vapor wherein accounting for cumulative volume 65 ~ 80% is sent into main heat exchanger re-heat to-140 ~-157 DEG C, cold is obtained again through expander, residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, carries out rectifying with the oxygen-enriched liquid air reflux sent in rectifying column through choke valve in step b;
Oxygen-enriched liquid air vapor in d, step c after expander enters main heat exchanger by re-heat again to normal temperature, in oxygen-enriched liquid air vapor after gained re-heat, a part accounts for the regeneration gas of cumulative volume 18 ~ 25% heater via heating as adsorbent in purifier, all the other emptying.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, be 81 ~ 83% from the volumn concentration of nitrogen in the nitrogenous waste gas of fractionating column system described in step a.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, air compressor described in step a is piston type air compressor or centrifugal air compressor; The next stage of air compressor described in step a entrance is secondary inlet, three grades of entrances or level Four entrance.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, enter purifier described in step a and purify, after purification, remove water, carbon dioxide, acetylene and other hydrocarbon.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, described main heat exchanger is multiple flow aluminum plate-fin heat exchanger.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, described lower rectifying column or upper rectifying column are the sieve-plate tower or regular packed tower that adopt cryogenic material or stainless steel material to make.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, the column plate form of described sieve-plate tower is convection current sieve-plate tower or circulation sieve-plate tower.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, described condenser/evaporator is thermosiphon evaporator.
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, decompressor described in step c comprises the turbo-expander of blower fan braking, the turbo-expander of oil brake, the turbo-expander of generator brake and gas bearing decompressor
;
The pressure of nitrogenous waste gas described in step c is 0.317 ~ 0.46 MPa(a).
According to above-mentioned utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, heater described in steps d is electric heater or steam heater.
The two-stage rectification system that the upper rectifying column C2 that the heat-exchange system that the fractionating column system adopted in technical solution of the present invention is at least made up of main heat exchanger E1, condenser/evaporator K1 connect as one and lower rectifying column C1 is formed and the refrigeration system that decompressor forms form.
The roughly technique that the present invention produces purity nitrogen is: first the purification unstripped gas entering fractionating column system is cooled to dew point (i.e. saturation temperature) by reflux gas in main heat exchanger E1, and has portion gas to be liquefied, and finally enters lower rectifying column C1 and carries out rectifying; Obtain the nitrogen being not more than 50ppm containing oxygen at lower rectifying column C1 top, lower rectifier bottoms obtains the oxygen-enriched liquid air containing oxygen about 33%.A nitrogen part of lower rectifying column top C1 is sent after main heat exchanger E1 re-heat as gas product, a part be cooled in condenser/evaporator K1 liquid carrying under the phegma of rectifying column C1 and nitrogen products; The oxygen-enriched liquid air of bottom enters rectifying column C2 and carries out rectifying.Obtain the nitrogenous waste gas of nitrogenous about 81% at upper rectifying column C2 top, bottom obtains the oxygen-enriched liquid air containing oxygen about 63%.Nitrogenous waste gas from upper rectifying column C2 enters a certain inter-stage import of air compressor machine TC in main heat exchanger E1 after re-heat, as unstripped gas after mixing with the raw air from air compressor machine TC.A part is as safety dumping in condenser/evaporator K1 for the oxygen-enriched liquid air that upper rectifying column C2 comes, and all the other are by the nitrogen heating evaporation of lower rectifying column C1, and a part is extracted out as expansion gas from upper rectifier bottoms, and a part is as the rising gas of upper rectifying column C2.
positive beneficial effect of the present invention:
1, technical solution of the present invention take to reclaim there is certain pressure the nitrogenous waste gas that backflows to a certain inter-stage entrance of air compressor, mix with the raw air through air compressor one-level entrance recompress, precooling, purification, finally liquefy in fractionating column system, rectifying produce nitrogen.Adopting technical solution of the present invention to produce purity nitrogen, can improve the recovery rate of nitrogen product, reduce the operation energy consumption of device, is the novel process that a kind of two stage rectification stream backed expansion produces nitrogen.
2, to mix the nitrogen concentration of the unstripped gas that improve into fractionating column system in technical solution of the present invention with raw air owing to having reclaimed waste gas from the nitrogen content 81 ~ 83% of fractionating column system, general technology enters that the unstripped gas of fractionating column is nitrogenous equals air nitrogenous 78%, utilize technical solution of the present invention to produce nitrogen and can reduce unstripped gas into fractionating column, improve the recovery rate of nitrogen product.
3, utilize technical solution of the present invention to produce nitrogen, reclaimed the waste gas that backflows with certain pressure from fractionating column system to a certain inter-stage entrance of air compressor, decreased the suction inlet flow of air compressor, thus reduce the energy consumption of air compressor.
4, technical solution of the present invention is utilized to produce nitrogen, for 1000 purity nitrogen equipment, go out equipment nitrogen pressure 0.8MPa(G), product nitrogen gas is containing oxygen 14ppm, liquid nitrogen is example containing oxygen 50ppm, nitrogen recovery rate brings up to 61% by traditional recovery rate 50%, and energy consumption is reduced to 0.284kWh/Nm3 N2 by 0.325 kWh/Nm3 N2, power saving 42KW per hour.It can thus be appreciated that technical solution of the present invention has significant economic benefit and social benefit.
four, accompanying drawing illustrates:
Fig. 1 the present invention utilize nitrogenous waste gas to carry out again process flow diagram that cryogenic rectification produces the method for purity nitrogen.
In Fig. 1: AF is air cleaner, TC is air compressor, and RU is Precooling unit, and MS is molecular sieve purifier, EH electric heater, and E1 is main heat exchanger, and K1 is condenser/evaporator, and C1 is lower rectifying column, and C2 is upper rectifying column, and ET is decompressor, and SL is silencer.
five, detailed description of the invention:
Set forth the present invention further below in conjunction with embodiment, but do not limit content of the present invention.
Embodiment 1:
See accompanying drawing 1, the present invention's utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, the detailed step of the method is as follows:
A, with 1000 purity nitrogen equipment for benchmark, produce purity nitrogen with air and from the nitrogenous waste gas of fractionating column system for unstripped gas, first by the first unstripped gas 2178Nm
3/ h air sends into air cleaner, dust in air cleaner removing air and impurity, then enter air compressor and be compressed into 0.46MPa(a), the pressure simultaneously from fractionating column system is 0.46MPa(a), nitrogen content is that the nitrogenous waste gas of the second unstripped gas of 82% is with 526Nm
3the intake of/h is vented with the inter-stage from air compressor carries out being mixed to get the 3rd unstripped gas with the first unstripped gas, 3rd unstripped gas enters air compressor compression from air compressor next stage entrance again, compression eventually last pressure is 1.0MPa(a), the 3rd unstripped gas after compression cools the temperature to 5 ~ 8 DEG C through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and purifies, water, carbon dioxide, acetylene and other hydrocarbon is removed, the 3rd unstripped gas after being purified after purification;
The 3rd unstripped gas after b, step a purification enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as upflowing vapor, is separated, obtains 2743Nm at lower rectifying column top through rectifying
3/ h nitrogen content 99.93%, pure nitrogen gas containing oxygen 13ppm, the 1000Nm in gained pure nitrogen gas
3/ h collects as product nitrogen gas to 5 ~ 7 DEG C through main heat exchanger re-heat; Residual income pure nitrogen gas is cooled to liquid nitrogen in condenser/evaporator, extracts 40Nm
3/ h liquid nitrogen can be used as nitrogen products and discharges collection, remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying is separated, obtain the oxygen-enriched liquid air 1664Nm3/h containing oxygen 32.8% in the bottom of lower rectifying column, gained oxygen-enriched liquid air sends into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air sending into upper rectifying column in c, step b is separated through rectifying, obtains the waste gas 526Nm3/h of nitrogenous 82% at upper rectifying column top, and the nitrogenous waste gas of gained sends into the inter-stage entrance of air compressor in step a as the second unstripped gas; The bottom of upper rectifying column obtains the oxygen enrichment 1450Nm containing oxygen 63.5%
3/ h, wherein 10Nm
3the oxygen enriched liquid of/h directly discharges fractionating column system, and as safety dumping, residue oxygen enriched liquid by the nitrogen heating and gasifying that lower rectifying column top obtains, obtains oxygen-enriched liquid air vapor 1441 Nm3/h containing oxygen 39.37% in condenser/evaporator; Extract 1128 Nm out
3the oxygen-enriched liquid air vapor of/h sends into main heat exchanger re-heat to-140 DEG C, cold is obtained again through expander, residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, carries out rectifying with the oxygen-enriched liquid air reflux sent in rectifying column through choke valve in step b;
Oxygen-enriched liquid air vapor in d, step c after expander enters main heat exchanger again by re-heat to normal temperature, about 450Nm
3/ h heats the regeneration gas as adsorbent in purifier through electric heater, all the other emptying.
Above-described embodiment 1 is according to nitrogen gas purity requirement, and 42 blocks of theoretical trays got by lower rectifying column, and 6 blocks of theoretical trays got by upper rectifying column; Upper rectifying column operating pressure 0.495MPa (a), lower rectifying column operating pressure 0.945MPa (a), the condenser/evaporator temperature difference 1.1 DEG C.
The detection data of embodiment 1 products obtained therefrom nitrogen purity refer to table 1.
Embodiment 2:
The present invention's utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, the detailed step of the method is as follows:
A, with 1000 purity nitrogen equipment for benchmark, produce purity nitrogen with air and from the nitrogenous waste gas of fractionating column system for unstripped gas, first by the first unstripped gas 2178Nm
3/ h air sends into air cleaner, dust in air cleaner removing air and impurity, then enter air compressor and be compressed into 0.46MPa(a), the pressure simultaneously from fractionating column system is 0.46MPa(a), the nitrogenous waste gas of the second unstripped gas of nitrogen content 81.9% is with 519Nm
3the intake of/h and the inter-stage from air compressor be vented and the first raw material its carry out being mixed to get the 3rd unstripped gas, 3rd unstripped gas enters air compressor compression from air compressor next stage entrance again, compression eventually last pressure is 1.0MPa(a), the 3rd unstripped gas after compression cools the temperature to 5 ~ 8 DEG C through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and purifies, water, carbon dioxide, acetylene and other hydrocarbon is removed, the 3rd unstripped gas after being purified after purification;
The 3rd unstripped gas after b, step a purification enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as upflowing vapor, is separated, obtains 2739Nm at lower rectifying column top through rectifying
3/ h nitrogen content 99.93%, pure nitrogen gas containing oxygen 0.597ppm, the 1000Nm in gained pure nitrogen gas
3/ h collects as product nitrogen gas to 5 ~ 7 DEG C through main heat exchanger re-heat; Residual income nitrogen is cooled to liquid nitrogen in condenser/evaporator, extracts 40Nm
3/ h liquid nitrogen can be used as product and discharges and collect, and remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying is separated, obtains the oxygen-enriched liquid air 1657Nm containing oxygen 32.9% in the bottom of lower rectifying column
3/ h, gained oxygen-enriched liquid air sends into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air sending into upper rectifying column in c, step b is separated through rectifying, obtains the waste gas 519Nm of nitrogenous 81.9% at upper rectifying column top
3/ h, the nitrogenous waste gas of gained sends into the inter-stage entrance of air compressor in step a as the second unstripped gas; The bottom of upper rectifying column obtains the oxygen enrichment 1446Nm containing oxygen 63.4%
3/ h, wherein 10Nm
3the oxygen enriched liquid of/h directly discharges fractionating column system, and as safety dumping, residue oxygen enriched liquid by the nitrogen heating and gasifying that lower rectifying column top obtains, obtains oxygen-enriched liquid air vapor 1441 Nm containing oxygen 39.9% in condenser/evaporator
3/ h; Extract 1128 Nm out
3the oxygen-enriched liquid air vapor of/h sends into main heat exchanger re-heat to-140 DEG C, cold is obtained again through expander, residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, carries out rectifying with the oxygen-enriched liquid air reflux sent in rectifying column through choke valve in step b;
Oxygen-enriched liquid air vapor in d, step c after expander enters main heat exchanger again by re-heat to normal temperature, about 450Nm
3/ h heats the regeneration gas as adsorbent in purifier through electric heater, all the other emptying.
Above-described embodiment 2 is according to nitrogen gas purity requirement, and 55 blocks of theoretical trays got by lower rectifying column, and 6 blocks of theoretical trays got by upper rectifying column; Upper rectifying column operating pressure 0.495MPa (a), lower rectifying column operating pressure 0.945MPa (a), the condenser/evaporator temperature difference 1.1 DEG C.
The detection data of embodiment 2 products obtained therefrom nitrogen purity refer to table 2.
Embodiment 3:
The present invention's utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, the detailed step of the method is as follows:
A, with 1000 purity nitrogen equipment for benchmark, produce purity nitrogen with air and from the nitrogenous waste gas of fractionating column system for unstripped gas, first by the first unstripped gas 2030Nm
3/ h air sends into air cleaner, dust in air cleaner removing air and impurity, then enter air compressor and be compressed into 0.193MPa(a), the pressure simultaneously from fractionating column system is that the nitrogenous waste gas of the second unstripped gas of 0.317MPa (a) is with 309Nm
3the intake of/h and the inter-stage from air compressor be vented and the first raw material its carry out being mixed to get the 3rd unstripped gas, 3rd unstripped gas enters air compressor compression from air compressor next stage entrance again, compression eventually last pressure is 0.75MPa (a), the 3rd unstripped gas after compression cools the temperature to 5 ~ 8 DEG C through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and purifies, water, carbon dioxide, acetylene and other hydrocarbon is removed, the 3rd unstripped gas after being purified after purification;
The 3rd unstripped gas after b, step a purification enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as upflowing vapor, is separated, obtains 2380Nm at lower rectifying column top through rectifying
3/ h nitrogen content 99.87%, pure nitrogen gas containing oxygen 11ppm, the 1000Nm in gained pure nitrogen gas
3/ h collects as product nitrogen gas to 5 ~ 7 DEG C through main heat exchanger re-heat; Residual income nitrogen is cooled into liquid nitrogen in condenser/evaporator, and under returning, rectifying column carries out rectifying as the phegma of lower rectifying column, after rectifying is separated, obtains the oxygen-enriched liquid air 1339Nm containing oxygen 34.7% in the bottom of lower rectifying column
3/ h, gained oxygen-enriched liquid air sends into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air sending into upper rectifying column in c, step b is separated through rectifying, obtains the waste gas 309Nm of nitrogenous 81.6% at upper rectifying column top
3/ h, the nitrogenous waste gas of gained sends into the inter-stage entrance of air compressor in step a as the second unstripped gas; The bottom of upper rectifying column obtains the oxygen enriched liquid 1186Nm containing oxygen 66.7%
3/ h, wherein 10Nm
3the oxygen enriched liquid of/h directly discharges fractionating column system, and as safety dumping, residue oxygen enriched liquid by the nitrogen heating and gasifying that lower rectifying column top obtains, obtains oxygen-enriched liquid air vapor 1176 Nm containing oxygen 40.9% in condenser/evaporator
3/ h; Extract 1020 Nm out
3the oxygen-enriched liquid air vapor of/h sends into main heat exchanger re-heat to-157 DEG C, cold is obtained again through expander, residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, carries out rectifying with the oxygen-enriched liquid air reflux sent in rectifying column through choke valve in step b;
Oxygen-enriched liquid air vapor in d, step c after expander enters main heat exchanger again by re-heat to normal temperature, about 450Nm
3/ h heats the regeneration gas as adsorbent in purifier through electric heater, all the other emptying.
Above-described embodiment 1 is according to nitrogen gas purity requirement, and 42 blocks of theoretical trays got by lower rectifying column, and 6 blocks of theoretical trays got by upper rectifying column; Upper rectifying column operating pressure 0.34MPa (a), lower rectifying column operating pressure 0.695MPa (a), the condenser/evaporator temperature difference 1.1 DEG C.
The detection data of embodiment 3 products obtained therefrom nitrogen purity refer to table 1.
Embodiment 4:
The present invention's utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen, the detailed step of the method is as follows:
A, with 1000 purity nitrogen equipment for benchmark, produce purity nitrogen with air and from the nitrogenous waste gas of fractionating column system for unstripped gas, first by the first unstripped gas 2030Nm
3/ h air sends into air cleaner, dust in air cleaner removing air and impurity, then enter air compressor and be compressed into 0.193MPa(a), the pressure simultaneously from fractionating column system is that the nitrogenous waste gas of the second unstripped gas of 0.317MPa (a) is with 309Nm
3the intake of/h and the inter-stage from air compressor be vented and the first raw material its carry out being mixed to get the 3rd unstripped gas, 3rd unstripped gas enters air compressor compression from air compressor next stage entrance again, compression eventually last pressure is 0.75MPa (a), the 3rd unstripped gas after compression cools the temperature to 5 ~ 8 DEG C through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and purifies, water, carbon dioxide, acetylene and other hydrocarbon is removed, the 3rd unstripped gas after being purified after purification;
The 3rd unstripped gas after b, step a purification enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as upflowing vapor, is separated, obtains 2380Nm at lower rectifying column top through rectifying
3/ h nitrogen content 99.91%, pure nitrogen gas containing oxygen 413ppb (0.413ppm), the 1000Nm in gained pure nitrogen gas
3/ h collects as product nitrogen gas to 5 ~ 7 DEG C through main heat exchanger re-heat; Residual income nitrogen is cooled into liquid nitrogen in condenser/evaporator, and under returning, rectifying column carries out rectifying as the phegma of lower rectifying column, after rectifying is separated, obtains the oxygen-enriched liquid air 1339Nm containing oxygen 34.7% in the bottom of lower rectifying column
3/ h, gained oxygen-enriched liquid air sends into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air sending into upper rectifying column in c, step b is separated through rectifying, obtains the waste gas 309Nm3/h of nitrogenous 81.6% at upper rectifying column top, and the nitrogenous waste gas of gained sends into the inter-stage entrance of air compressor in step a as the second unstripped gas; The bottom of upper rectifying column obtains the oxygen enriched liquid 1186Nm containing oxygen 66.7%
3/ h, wherein 10Nm
3the oxygen enriched liquid of/h directly discharges fractionating column system, and as safety dumping, residue oxygen enriched liquid by the nitrogen heating and gasifying that lower rectifying column top obtains, obtains oxygen-enriched liquid air vapor 1176 Nm containing oxygen 40.9% in condenser/evaporator
3/ h; Extract 1020 Nm out
3the oxygen-enriched liquid air vapor of/h sends into main heat exchanger re-heat to-157 DEG C, cold is obtained again through expander, residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, carries out rectifying with the oxygen-enriched liquid air reflux sent in rectifying column through choke valve in step b;
Oxygen-enriched liquid air vapor in d, step c after expander enters main heat exchanger again by re-heat to normal temperature, about 450Nm
3/ h heats the regeneration gas as adsorbent in purifier through electric heater, all the other emptying.
Above-described embodiment 1 is according to nitrogen gas purity requirement, and 55 blocks of theoretical trays got by lower rectifying column, and 6 blocks of theoretical trays got by upper rectifying column; Upper rectifying column operating pressure 0.34MPa (a), lower rectifying column operating pressure 0.695MPa (a), the condenser/evaporator temperature difference 1.1 DEG C.
The detection data of embodiment 4 products obtained therefrom nitrogen purity refer to table 1.
The above embodiment of the present invention, by increasing the method such as theoretical cam curve of air capacity, lower rectifying column, can obtain more highly purified nitrogen.
Claims (1)
1. utilize nitrogenous waste gas to carry out an again method that cryogenic rectification produces purity nitrogen, is characterized in that, said method comprising the steps of:
A, with 1000 purity nitrogen equipment for benchmark, produce purity nitrogen using air as the first unstripped gas, from the nitrogenous waste gas of fractionating column system as the second unstripped gas, first by the first unstripped gas air with 2000 ~ 2200Nm
3the intake of/h sends into air cleaner, dust in air cleaner removing air and impurity, then enter air compressor and be compressed into 0.19 ~ 0.46 MPa(a), the pressure simultaneously from fractionating column system is 0.317 ~ 0.46 MPa(a) the nitrogenous waste gas of the second unstripped gas with 300 ~ 550 Nm
3the intake of/h enters air compressor and the first unstripped gas carries out being mixed to get the 3rd unstripped gas, 3rd unstripped gas enters air compressor from air compressor next stage entrance again and compresses, compression eventually last pressure is 0.75 ~ 1.1 MPa(a), the 3rd unstripped gas after compression cools the temperature to 5 ~ 8 DEG C through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and purifies, the 3rd unstripped gas after being purified;
The 3rd unstripped gas after b, step a purification enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as upflowing vapor, is separated, obtains 2300 ~ 2780 Nm at lower rectifying column top through rectifying
3the pure nitrogen gas of/h, in gained pure nitrogen gas 35 ~ 45% DEG C to collect as product nitrogen gas through main heat exchanger re-heat to 5 ~ 7; Residual income pure nitrogen gas is cooled to liquid nitrogen in condenser/evaporator, the gained liquid nitrogen of wherein≤4% is discharged as nitrogen products and is collected, remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying is separated, obtain oxygen-enriched liquid air 1300 ~ 1700 Nm containing oxygen 32 ~ 35% in the bottom of lower rectifying column
3/ h, gained oxygen-enriched liquid air sends into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air sending into upper rectifying column in c, step b is separated through rectifying, obtains waste gas 300 ~ 550 Nm of nitrogenous volumn concentration 81 ~ 83% at upper rectifying column top
3/ h, the nitrogenous waste gas of gained sends into the inter-stage entrance of air compressor in step a as the second unstripped gas; The bottom of upper rectifying column obtains oxygen enriched liquid 1100 ~ 1560 Nm containing oxygen 62 ~ 67%
3/ h, the oxygen enriched liquid wherein accounting for gained oxygen enrichment volume 0.5 ~ 0.8% directly discharges fractionating column system, as safety dumping, residue oxygen enriched liquid by the nitrogen heating and gasifying that lower rectifying column top obtains, obtains the oxygen-enriched liquid air vapor containing oxygen 38 ~ 41% in condenser/evaporator; The oxygen-enriched liquid air vapor wherein accounting for cumulative volume 65 ~ 80% is sent into main heat exchanger re-heat to-140 ~-157 DEG C, cold is obtained again through expander, residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, carries out rectifying with the oxygen-enriched liquid air reflux sent in rectifying column through choke valve in step b;
Oxygen-enriched liquid air vapor in d, step c after expander enters main heat exchanger by re-heat again to normal temperature, in oxygen-enriched liquid air vapor after gained re-heat, a part accounts for the regeneration gas of cumulative volume 18 ~ 25% heater via heating as adsorbent in purifier, all the other emptying.
2. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, is characterized in that: be 81 ~ 83% from the volumn concentration of nitrogen in the nitrogenous waste gas of fractionating column system described in step a.
3. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, is characterized in that: air compressor described in step a is piston type air compressor or centrifugal air compressor; The next stage of air compressor described in step a entrance is secondary inlet, three grades of entrances or level Four entrance.
4. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, it is characterized in that: the 3rd unstripped gas after cooling described in step a enters purifier and purifies, and removes water, carbon dioxide, acetylene and other hydrocarbon after purification.
5. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, is characterized in that: described main heat exchanger is multiple flow aluminum plate-fin heat exchanger.
6. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, is characterized in that: described lower rectifying column or upper rectifying column are the sieve-plate tower or regular packed tower that adopt cryogenic material to make.
7. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 6, is characterized in that: the column plate form of described sieve-plate tower is convection current sieve-plate tower or circulation sieve-plate tower.
8. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, is characterized in that: described condenser/evaporator is thermosiphon evaporator.
9. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, is characterized in that: decompressor described in step c comprises the turbo-expander of blower fan braking, the turbo-expander of oil brake, the turbo-expander of generator brake and gas bearing decompressor
;
The pressure of nitrogenous waste gas described in step c is 0.317 ~ 0.46 MPa(a).
10. utilize nitrogenous waste gas to carry out again method that cryogenic rectification produces purity nitrogen according to claim 1, is characterized in that: heater described in steps d is electric heater or steam heater.
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| CN114165988B (en) * | 2021-11-22 | 2023-01-31 | 四川空分设备(集团)有限责任公司 | Low-pressure nitrogen preparation device and method |
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