CN103123203A - 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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- CN103123203A CN103123203A CN201310056697XA CN201310056697A CN103123203A CN 103123203 A CN103123203 A CN 103123203A CN 201310056697X A CN201310056697X A CN 201310056697XA CN 201310056697 A CN201310056697 A CN 201310056697A CN 103123203 A CN103123203 A CN 103123203A
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- nitrogen
- oxygen
- gas
- enriched liquid
- rectifying column
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 269
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 120
- 239000007789 gas Substances 0.000 title claims abstract description 98
- 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 107
- 239000001301 oxygen Substances 0.000 claims abstract description 107
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 107
- 239000007788 liquid Substances 0.000 claims abstract description 94
- 230000000630 rising effect Effects 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 7
- 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 29
- 230000006835 compression Effects 0.000 claims description 17
- 238000007906 compression Methods 0.000 claims description 17
- 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
- 239000000463 material Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel 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
- 239000000284 extract Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 238000001514 detection method Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 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
- 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
- 239000002808 molecular sieve Substances 0.000 description 1
- 229940007041 oxygen 33 % Drugs 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
Classifications
-
- 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 of producing nitrogen, belong to the cryogenic air separation field, especially relate to and a kind ofly utilize nitrogenous waste gas to carry out the method for cryogenic rectification purity nitrogen processed again.
Background technology
Along with socioeconomic development, in recent years, produce the air separation plant application of nitrogen and constantly expand, and to the higher requirement of 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 tradition cryogenic rectification legal system nitrogen has two kinds of single-stage rectifying waste expansion flow process and single-stage rectifying air expansion flow processs.Wherein, single-stage rectifying waste expansion product nitrogen gas pressure, at 0.45～0.9MPa, is directly given the user and is used after the product nitrogen gas cooling box, and the nitrogen product recovery rate is generally 45%～58%; Single-stage rectifying air expansion product nitrogen gas pressure is at 0.175～1.35MPa, and the 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 two kinds of techniques of single-stage rectifying air expansion flow process is low, energy consumption is high the invention provides and a kind ofly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen again.Technical solution of the present invention is taked to reclaim has the nitrogenous waste gas of backflowing of certain pressure to three grades of entrances of air compressor, with raw air mixing recompression, precooling, the purification through the air compressor two-stage compression, finally in fractionating column system, nitrogen is produced in liquefaction, rectifying.Adopting technical solution of the present invention to produce purity nitrogen, can improve the recovery rate of nitrogen product, the operation energy consumption of reduction device, is the technique that a kind of novel stream backed expansion is produced nitrogen.
In order to address the above problem, the technical solution used in the present invention is:
The invention provides and a kind ofly utilize nitrogenous waste gas to carry out again the method that cryogenic rectification is produced purity nitrogen, said method comprising the steps of:
A, the 1000 purity nitrogen equipment of take are benchmark, produce purity nitrogen and using air as the first unstripped gas, from the nitrogenous waste gas of fractionating column system as the second unstripped gas, at first by the first unstripped gas air with 2000～2200Nm
3the intake of/h is sent into air cleaner, remove airborne dust and impurity through air cleaner, then enter air compressor and be compressed into 0.19～0.46 MPa(a), simultaneously the pressure 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 is mixed to get the 3rd unstripped gas, the 3rd unstripped gas enters air compressor from air compressor next stage entrance again and is compressed, compression last pressure eventually is 0.75～1.1 MPa(a), the 3rd unstripped gas after compression cools the temperature to 5～8 ℃ through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and is purified, the 3rd unstripped gas after being purified;
The 3rd unstripped gas after b, step a purify enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as rising steam, through rectifying, separates, and at lower rectifying column top, obtains 2300～2780 Nm
3the pure nitrogen gas of/h, 35～45% in the gained pure nitrogen gas ℃ collected as product nitrogen gas through main heat exchanger re-heat to 5～7; The residual income pure nitrogen gas is cooled to liquid nitrogen in condenser/evaporator, wherein≤4% gained liquid nitrogen is discharged and is collected as nitrogen products, the remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying separates, obtain oxygen-enriched liquid air 1300～1700 Nm containing oxygen 32～35% in the bottom of lower rectifying column
3/ h, the gained oxygen-enriched liquid air is sent into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air of sending into rectifying column in c, step b separates 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 is sent into the inter-stage entrance of step a Air compressor 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 that wherein accounts for gained oxygen enrichment volume 0.5～0.8% is directly discharged fractionating column system, as safety dumping, the residue oxygen enriched liquid nitrogen heating and gasifying that under quilt, the rectifying column top obtains in condenser/evaporator, obtain the oxygen-enriched liquid air vapor containing oxygen 38～41%; The oxygen-enriched liquid air vapor that wherein accounts for cumulative volume 65～80% is sent into to the main heat exchanger re-heat to-140～-157 ℃, expand and obtain cold through decompressor again, the residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, with the oxygen-enriched liquid air reflux of sending in upper rectifying column through choke valve in step b, carries out rectifying;
Oxygen-enriched liquid air vapor in d, step c after decompressor expands again enter main heat exchanger by re-heat to normal temperature, in oxygen-enriched liquid air vapor after the 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.
Carry out according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, the volumn concentration from nitrogen in the nitrogenous waste gas of fractionating column system described in step a is 81～83% again.
Carry out according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, air compressor described in step a is piston type air compressor or centrifugal air compressor again; The next stage of air compressor described in step a entrance is secondary entrance, three grades of entrances or level Four entrance.
Carry out again according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, enter purifier described in step a and purified, after purifying, remove water, carbon dioxide, acetylene and other hydrocarbon.
Carry out according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, described main heat exchanger is the multiple flow aluminum plate-fin heat exchanger again.
Carry out again according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, described lower rectifying column or upper rectifying column sieve-plate tower or the regular packed tower for adopting cryogenic material or stainless steel material to make.
Carry out according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, the column plate form of described sieve-plate tower is convection current sieve-plate tower or circulation sieve-plate tower again.
Carry out according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, described condenser/evaporator is the thermal siphon evaporimeter again.
Carry out according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, decompressor described in step c comprises the turbo-expander of blower fan braking, the turbo-expander of oil brake, turbo-expander and the gas bearing decompressor of generator brake again
;
The pressure of nitrogenous waste gas described in step c is 0.317～0.46 MPa(a).
Carry out according to the above-mentioned nitrogenous waste gas that utilizes the method that cryogenic rectification is produced purity nitrogen, heater described in steps d is electric heater or steam heater again.
The refrigeration system that 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 at least is comprised of main heat exchanger E1, condenser/evaporator K1 connect as one and lower rectifying column C1 form and decompressor form forms.
The roughly technique that the present invention produces purity nitrogen is: at first the purification unstripped gas that enters fractionating column system is cooled to dew point (being saturation temperature) by anti-gas body in main heat exchanger E1, and has portion gas to be liquefied, and finally enters lower rectifying column C1 and carries out rectifying; Obtain being not more than containing oxygen the nitrogen of 50ppm at lower rectifying column C1 top, lower rectifier bottoms obtains the oxygen-enriched liquid air containing oxygen 33% left and right.The nitrogen part of lower rectifying column top C1 is sent after main heat exchanger E1 re-heat as gas product, and a part is cooled into phegma and the nitrogen products of rectifying column C1 under the liquid carrying confession in condenser/evaporator K1; The oxygen-enriched liquid air of bottom enters rectifying column C2 and carries out rectifying.Obtain the nitrogenous waste gas of nitrogenous 81% left and right at upper rectifying column C2 top, bottom obtains the oxygen-enriched liquid air containing oxygen 63% left and right.Enter a certain inter-stage import of air compressor machine TC after re-heat in main heat exchanger E1 from the nitrogenous waste gas of upper rectifying column C2, with after raw air from air compressor machine TC mixes as unstripped gas.The oxygen-enriched liquid air that upper rectifying column C2 comes in condenser/evaporator K1 a part as safety dumping, all the other heating evaporations of the nitrogen by lower rectifying column C1, a part from rectifier bottoms extract out as expansion gas, 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 is taked to reclaim and is had the nitrogenous waste gas of backflowing of certain pressure to a certain inter-stage entrance of air compressor, with raw air mixing recompression, precooling, the purification through air compressor one-level entrance, finally in fractionating column system, nitrogen is produced in liquefaction, rectifying.Adopting technical solution of the present invention to produce purity nitrogen, can improve the recovery rate of nitrogen product, the operation energy consumption of reduction device, is the novel process that a kind of two stage rectification stream backed expansion is produced nitrogen.
2, in technical solution of the present invention because the waste gas reclaimed from the nitrogen content 81～83% of fractionating column system mixes the nitrogen concentration of the unstripped gas that has improved fractionating column system with raw air, general technology enters the nitrogenous atmosphere nitrogenous 78% that equals of unstripped gas of fractionating column, utilize technical solution of the present invention to produce nitrogen and can reduce the 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, reduced the suction inlet flow of air compressor, thereby reduced the energy consumption of air compressor.
4, utilize technical solution of the present invention to produce nitrogen, the 1000 purity nitrogen equipment of take are example, go out equipment nitrogen pressure 0.8MPa(G), product nitrogen gas is containing oxygen 14ppm, liquid nitrogen is example containing oxygen 50ppm, the 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, per hour power saving 42KW.Hence one can see that, and technical solution of the present invention has significant economic benefit and social benefit.
four, accompanying drawing explanation:
Fig. 1 the present invention utilizes nitrogenous waste gas to carry out the process flow diagram that cryogenic rectification is produced the method for purity nitrogen again.
In Fig. 1: AF is air cleaner, and TC is air compressor, and RU is Precooling unit, and MS is molecular sieve purifier, the 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, the specific embodiment:
Further set forth the present invention below in conjunction with embodiment, but do not limit content of the present invention.
Embodiment 1:
Referring to accompanying drawing 1, the present invention utilizes nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen again, and the detailed step of the method is as follows:
A, the 1000 purity nitrogen equipment of take are benchmark, produce purity nitrogen and take air and be unstripped gas from the nitrogenous waste gas of fractionating column system, at first by the first unstripped gas 2178Nm
3/ h air is sent into air cleaner, remove airborne dust and impurity through air cleaner, then enter air compressor and be compressed into 0.46MPa(a), simultaneously the pressure from fractionating column system is 0.46MPa(a), the nitrogen content nitrogenous waste gas of the second unstripped gas that is 82% is with 526Nm
3the intake of/h is mixed to get the 3rd unstripped gas with inter-stage exhaust and the first unstripped gas from air compressor, the 3rd unstripped gas enters the air compressor compression from air compressor next stage entrance again, compression last pressure eventually is 1.0MPa(a), the 3rd unstripped gas after compression cools the temperature to 5～8 ℃ through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and is purified, remove water, carbon dioxide, acetylene and other hydrocarbon, the 3rd unstripped gas after being purified after purifying;
The 3rd unstripped gas after b, step a purify enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as rising steam, through rectifying, separates, and at lower rectifying column top, obtains 2743Nm
3/ h nitrogen content 99.93%, containing the pure nitrogen gas of oxygen 13ppm, the 1000Nm in the gained pure nitrogen gas
3/ h ℃ collects as product nitrogen gas through main heat exchanger re-heat to 5 ~ 7; The 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, the remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying separates, obtain the oxygen-enriched liquid air 1664Nm3/h containing oxygen 32.8% in the bottom of lower rectifying column, the gained oxygen-enriched liquid air is sent into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air of sending into rectifying column in c, step b separates through rectifying, obtains nitrogenous 82% waste gas 526Nm3/h at upper rectifying column top, and the nitrogenous waste gas of gained is sent into the inter-stage entrance of step a Air compressor 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 is directly discharged fractionating column system, and as safety dumping, the residue oxygen enriched liquid nitrogen heating and gasifying that under quilt, the rectifying column top obtains in condenser/evaporator, obtain oxygen-enriched liquid air vapor 1441 Nm3/h containing oxygen 39.37%; Extract 1128 Nm out
3the oxygen-enriched liquid air vapor of/h is sent into the main heat exchanger re-heat to-140 ℃, expand and obtain cold through decompressor again, the residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, with the oxygen-enriched liquid air reflux of sending in upper rectifying column through choke valve in step b, carries out rectifying;
Oxygen-enriched liquid air vapor in d, step c after decompressor expands again enter main heat exchanger by re-heat to normal temperature, about 450Nm
3the regeneration gas of/h adsorbent in electric heater heats as purifier, all the other emptying.
Above-described embodiment 1 is according to the nitrogen gas purity requirement, and lower rectifying column is got 42 blocks of theoretical trays, and upper rectifying column is got 6 blocks of theoretical trays; Upper rectifying column operating pressure 0.495MPa (a), lower rectifying column operating pressure 0.945MPa (a), 1.1 ℃ of the condenser/evaporator temperature difference.
The detection data of embodiment 1 products obtained therefrom nitrogen purity refer to table 1.
Embodiment 2:
The present invention utilizes nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen again, and the detailed step of the method is as follows:
A, the 1000 purity nitrogen equipment of take are benchmark, produce purity nitrogen and take air and be unstripped gas from the nitrogenous waste gas of fractionating column system, at first by the first unstripped gas 2178Nm
3/ h air is sent into air cleaner, remove airborne dust and impurity through air cleaner, then enter air compressor and be compressed into 0.46MPa(a), simultaneously the pressure 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 is with from the inter-stage exhaust of air compressor and the first raw material, it is mixed to get the 3rd unstripped gas, the 3rd unstripped gas enters the air compressor compression from air compressor next stage entrance again, compression last pressure eventually is 1.0MPa(a), the 3rd unstripped gas after compression cools the temperature to 5～8 ℃ through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and is purified, remove water, carbon dioxide, acetylene and other hydrocarbon, the 3rd unstripped gas after being purified after purifying;
The 3rd unstripped gas after b, step a purify enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as rising steam, through rectifying, separates, and at lower rectifying column top, obtains 2739Nm
3/ h nitrogen content 99.93%, containing the pure nitrogen gas of oxygen 0.597ppm, the 1000Nm in the gained pure nitrogen gas
3/ h ℃ collects as product nitrogen gas through main heat exchanger re-heat to 5 ~ 7; Residual income nitrogen is cooled to liquid nitrogen in condenser/evaporator, extracts 40Nm
3/ h liquid nitrogen can be used as product and discharge to collect, and the remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying separates, obtains the oxygen-enriched liquid air 1657Nm containing oxygen 32.9% in the bottom of lower rectifying column
3/ h, the gained oxygen-enriched liquid air is sent into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air of sending into rectifying column in c, step b separates through rectifying, obtains nitrogenous 81.9% waste gas 519Nm at upper rectifying column top
3/ h, the nitrogenous waste gas of gained is sent into the inter-stage entrance of step a Air compressor 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 is directly discharged fractionating column system, and as safety dumping, the residue oxygen enriched liquid nitrogen heating and gasifying that under quilt, the rectifying column top obtains in condenser/evaporator, obtain oxygen-enriched liquid air vapor 1441 Nm containing oxygen 39.9%
3/ h; Extract 1128 Nm out
3the oxygen-enriched liquid air vapor of/h is sent into the main heat exchanger re-heat to-140 ℃, expand and obtain cold through decompressor again, the residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, with the oxygen-enriched liquid air reflux of sending in upper rectifying column through choke valve in step b, carries out rectifying;
Oxygen-enriched liquid air vapor in d, step c after decompressor expands again enter main heat exchanger by re-heat to normal temperature, about 450Nm
3the regeneration gas of/h adsorbent in electric heater heats as purifier, all the other emptying.
Above-described embodiment 2 is according to the nitrogen gas purity requirement, and lower rectifying column is got 55 blocks of theoretical trays, and upper rectifying column is got 6 blocks of theoretical trays; Upper rectifying column operating pressure 0.495MPa (a), lower rectifying column operating pressure 0.945MPa (a), 1.1 ℃ of the condenser/evaporator temperature difference.
The detection data of embodiment 2 products obtained therefrom nitrogen purity refer to table 2.
Embodiment 3:
The present invention utilizes nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen again, and the detailed step of the method is as follows:
A, the 1000 purity nitrogen equipment of take are benchmark, produce purity nitrogen and take air and be unstripped gas from the nitrogenous waste gas of fractionating column system, at first by the first unstripped gas 2030Nm
3/ h air is sent into air cleaner, remove airborne dust and impurity through air cleaner, then enter air compressor and be compressed into 0.193MPa(a), the nitrogenous waste gas of the second unstripped gas that is simultaneously 0.317MPa (a) from the pressure of fractionating column system is with 309Nm
3the intake of/h is with from the inter-stage exhaust of air compressor and the first raw material, it is mixed to get the 3rd unstripped gas, the 3rd unstripped gas enters the air compressor compression from air compressor next stage entrance again, compression last pressure eventually is 0.75MPa (a), the 3rd unstripped gas after compression cools the temperature to 5～8 ℃ through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and is purified, remove water, carbon dioxide, acetylene and other hydrocarbon, the 3rd unstripped gas after being purified after purifying;
The 3rd unstripped gas after b, step a purify enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as rising steam, through rectifying, separates, and at lower rectifying column top, obtains 2380Nm
3/ h nitrogen content 99.87%, containing the pure nitrogen gas of oxygen 11ppm, the 1000Nm in the gained pure nitrogen gas
3/ h ℃ collects as product nitrogen gas through main heat exchanger re-heat to 5 ~ 7; 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 separates, obtains the oxygen-enriched liquid air 1339Nm containing oxygen 34.7% in the bottom of lower rectifying column
3/ h, the gained oxygen-enriched liquid air is sent into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air of sending into rectifying column in c, step b separates through rectifying, obtains nitrogenous 81.6% waste gas 309Nm at upper rectifying column top
3/ h, the nitrogenous waste gas of gained is sent into the inter-stage entrance of step a Air compressor 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 is directly discharged fractionating column system, and as safety dumping, the residue oxygen enriched liquid nitrogen heating and gasifying that under quilt, the rectifying column top obtains in condenser/evaporator, obtain oxygen-enriched liquid air vapor 1176 Nm containing oxygen 40.9%
3/ h; Extract 1020 Nm out
3the oxygen-enriched liquid air vapor of/h is sent into the main heat exchanger re-heat to-157 ℃, expand and obtain cold through decompressor again, the residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, with the oxygen-enriched liquid air reflux of sending in upper rectifying column through choke valve in step b, carries out rectifying;
Oxygen-enriched liquid air vapor in d, step c after decompressor expands again enter main heat exchanger by re-heat to normal temperature, about 450Nm
3the regeneration gas of/h adsorbent in electric heater heats as purifier, all the other emptying.
Above-described embodiment 1 is according to the nitrogen gas purity requirement, and lower rectifying column is got 42 blocks of theoretical trays, and upper rectifying column is got 6 blocks of theoretical trays; Upper rectifying column operating pressure 0.34MPa (a), lower rectifying column operating pressure 0.695MPa (a), 1.1 ℃ of the condenser/evaporator temperature difference.
The detection data of embodiment 3 products obtained therefrom nitrogen purity refer to table 1.
Embodiment 4:
The present invention utilizes nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen again, and the detailed step of the method is as follows:
A, the 1000 purity nitrogen equipment of take are benchmark, produce purity nitrogen and take air and be unstripped gas from the nitrogenous waste gas of fractionating column system, at first by the first unstripped gas 2030Nm
3/ h air is sent into air cleaner, remove airborne dust and impurity through air cleaner, then enter air compressor and be compressed into 0.193MPa(a), the nitrogenous waste gas of the second unstripped gas that is simultaneously 0.317MPa (a) from the pressure of fractionating column system is with 309Nm
3the intake of/h is with from the inter-stage exhaust of air compressor and the first raw material, it is mixed to get the 3rd unstripped gas, the 3rd unstripped gas enters the air compressor compression from air compressor next stage entrance again, compression last pressure eventually is 0.75MPa (a), the 3rd unstripped gas after compression cools the temperature to 5～8 ℃ through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and is purified, remove water, carbon dioxide, acetylene and other hydrocarbon, the 3rd unstripped gas after being purified after purifying;
The 3rd unstripped gas after b, step a purify enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as rising steam, through rectifying, separates, and at lower rectifying column top, obtains 2380Nm
3/ h nitrogen content 99.91%, containing the pure nitrogen gas of oxygen 413ppb (0.413ppm), the 1000Nm in the gained pure nitrogen gas
3/ h ℃ collects as product nitrogen gas through main heat exchanger re-heat to 5 ~ 7; 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 separates, obtains the oxygen-enriched liquid air 1339Nm containing oxygen 34.7% in the bottom of lower rectifying column
3/ h, the gained oxygen-enriched liquid air is sent into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air of sending into rectifying column in c, step b separates through rectifying, obtains nitrogenous 81.6% waste gas 309Nm3/h at upper rectifying column top, and the nitrogenous waste gas of gained is sent into the inter-stage entrance of step a Air compressor 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 is directly discharged fractionating column system, and as safety dumping, the residue oxygen enriched liquid nitrogen heating and gasifying that under quilt, the rectifying column top obtains in condenser/evaporator, obtain oxygen-enriched liquid air vapor 1176 Nm containing oxygen 40.9%
3/ h; Extract 1020 Nm out
3the oxygen-enriched liquid air vapor of/h is sent into the main heat exchanger re-heat to-157 ℃, expand and obtain cold through decompressor again, the residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, with the oxygen-enriched liquid air reflux of sending in upper rectifying column through choke valve in step b, carries out rectifying;
Oxygen-enriched liquid air vapor in d, step c after decompressor expands again enter main heat exchanger by re-heat to normal temperature, about 450Nm
3the regeneration gas of/h adsorbent in electric heater heats as purifier, all the other emptying.
Above-described embodiment 1 is according to the nitrogen gas purity requirement, and lower rectifying column is got 55 blocks of theoretical trays, and upper rectifying column is got 6 blocks of theoretical trays; Upper rectifying column operating pressure 0.34MPa (a), lower rectifying column operating pressure 0.695MPa (a), 1.1 ℃ of the condenser/evaporator temperature difference.
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 methods such as theoretical cam curve of air capacity, lower rectifying column, can obtain more highly purified nitrogen.
Claims (10)
1. one kind is utilized nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen again, it is characterized in that, said method comprising the steps of:
A, the 1000 purity nitrogen equipment of take are benchmark, produce purity nitrogen and using air as the first unstripped gas, from the nitrogenous waste gas of fractionating column system as the second unstripped gas, at first by the first unstripped gas air with 2000～2200Nm
3the intake of/h is sent into air cleaner, remove airborne dust and impurity through air cleaner, then enter air compressor and be compressed into 0.19～0.46 MPa(a), simultaneously the pressure 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 is mixed to get the 3rd unstripped gas, the 3rd unstripped gas enters air compressor from air compressor next stage entrance again and is compressed, compression last pressure eventually is 0.75～1.1 MPa(a), the 3rd unstripped gas after compression cools the temperature to 5～8 ℃ through Precooling unit again and separates free water, the 3rd unstripped gas after cooling enters purifier and is purified, the 3rd unstripped gas after being purified;
The 3rd unstripped gas after b, step a purify enters main heat exchanger and is cooled to saturation temperature, then enters lower rectifying column and participates in rectifying as rising steam, through rectifying, separates, and at lower rectifying column top, obtains 2300～2780 Nm
3the pure nitrogen gas of/h, 35～45% in the gained pure nitrogen gas ℃ collected as product nitrogen gas through main heat exchanger re-heat to 5～7; The residual income pure nitrogen gas is cooled to liquid nitrogen in condenser/evaporator, wherein≤4% gained liquid nitrogen is discharged and is collected as nitrogen products, the remainder liquid nitrogen returns lower rectifying column and carries out rectifying as the phegma of lower rectifying column, after rectifying separates, obtain oxygen-enriched liquid air 1300～1700 Nm containing oxygen 32～35% in the bottom of lower rectifying column
3/ h, the gained oxygen-enriched liquid air is sent into the phegma of upper rectifying column as upper rectifying column through choke valve;
The oxygen-enriched liquid air of sending into rectifying column in c, step b separates 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 is sent into the inter-stage entrance of step a Air compressor 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 that wherein accounts for gained oxygen enrichment volume 0.5～0.8% is directly discharged fractionating column system, as safety dumping, the residue oxygen enriched liquid nitrogen heating and gasifying that under quilt, the rectifying column top obtains in condenser/evaporator, obtain the oxygen-enriched liquid air vapor containing oxygen 38～41%; The oxygen-enriched liquid air vapor that wherein accounts for cumulative volume 65～80% is sent into to the main heat exchanger re-heat to-140～-157 ℃, expand and obtain cold through decompressor again, the residue oxygen-enriched liquid air vapor enters upper rectifying column as rising gas and participates in rectifying, with the oxygen-enriched liquid air reflux of sending in upper rectifying column through choke valve in step b, carries out rectifying;
Oxygen-enriched liquid air vapor in d, step c after decompressor expands again enter main heat exchanger by re-heat to normal temperature, in oxygen-enriched liquid air vapor after the 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. according to claim 1ly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: the volumn concentration from nitrogen in the nitrogenous waste gas of fractionating column system described in step a is 81～83% again.
3. according to claim 1ly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: air compressor described in step a is piston type air compressor or centrifugal air compressor again; The next stage of air compressor described in step a entrance is secondary entrance, three grades of entrances or level Four entrance.
4. according to claim 1ly utilize nitrogenous waste gas to carry out again the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: enter purifier described in step a and purified, after purifying, remove water, carbon dioxide, acetylene and other hydrocarbon.
5. according to claim 1ly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: described main heat exchanger is the multiple flow aluminum plate-fin heat exchanger again.
6. according to claim 1ly utilize nitrogenous waste gas to carry out again the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: described lower rectifying column or upper rectifying column sieve-plate tower or the regular packed tower for adopting cryogenic material or stainless steel material to make.
7. according to claim 6ly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: the column plate form of described sieve-plate tower is convection current sieve-plate tower or circulation sieve-plate tower again.
8. according to claim 1ly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: described condenser/evaporator is the thermal siphon evaporimeter again.
9. according to claim 1ly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen again, it is characterized in that: decompressor described in step c comprises the turbo-expander of blower fan braking, the turbo-expander of oil brake, turbo-expander and the gas bearing decompressor of generator brake
;
The pressure of nitrogenous waste gas described in step c is 0.317～0.46 MPa(a).
10. according to claim 1ly utilize nitrogenous waste gas to carry out the method that cryogenic rectification is produced purity nitrogen, it is characterized in that: heater described in steps d is electric heater or steam heater again.
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| CN113623943A (en) * | 2021-08-22 | 2021-11-09 | 张家港市东南气体灌装有限公司 | Nitrogen manufacturing system and method for manufacturing nitrogen with different purities |
| CN113790575A (en) * | 2021-09-17 | 2021-12-14 | 东台宏仁气体有限公司 | High-purity oxygen manufacturing device and preparation method thereof |
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Denomination of invention: Method of producing pure nitrogen by cryogenic distillation of nitrogen containing waste gas Effective date of registration: 20220929 Granted publication date: 20150304 Pledgee: Bank of China Limited by Share Ltd. Kaifeng branch Pledgor: HENAN KAIYUAN AIR SEPARATION GROUP Co.,Ltd. Registration number: Y2022980016919 |
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Date of cancellation: 20231012 Granted publication date: 20150304 Pledgee: Bank of China Limited by Share Ltd. Kaifeng branch Pledgor: HENAN KAIYUAN AIR SEPARATION GROUP Co.,Ltd. Registration number: Y2022980016919 |