CN111482084B - Method for recycling nitrogen in flare gas of polyethylene device - Google Patents
Method for recycling nitrogen in flare gas of polyethylene device Download PDFInfo
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- CN111482084B CN111482084B CN202010448727.1A CN202010448727A CN111482084B CN 111482084 B CN111482084 B CN 111482084B CN 202010448727 A CN202010448727 A CN 202010448727A CN 111482084 B CN111482084 B CN 111482084B
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 216
- 239000007789 gas Substances 0.000 title claims abstract description 185
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 108
- -1 polyethylene Polymers 0.000 title claims abstract description 69
- 239000004698 Polyethylene Substances 0.000 title claims abstract description 66
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000004064 recycling Methods 0.000 title claims abstract description 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 95
- 238000000926 separation method Methods 0.000 claims abstract description 89
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 68
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 52
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 52
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 49
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 230000003197 catalytic effect Effects 0.000 claims abstract description 26
- 238000003795 desorption Methods 0.000 claims abstract description 23
- 238000007872 degassing Methods 0.000 claims abstract description 22
- 239000012528 membrane Substances 0.000 claims description 69
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 33
- 239000005977 Ethylene Substances 0.000 claims description 33
- 239000003463 adsorbent Substances 0.000 claims description 28
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 7
- 239000012466 permeate Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical class [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 238000009792 diffusion process Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000006096 absorbing agent Substances 0.000 description 22
- 239000003054 catalyst Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000011010 flushing procedure Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- XTEXMYNJEMCTNI-UHFFFAOYSA-N ethene;methane Chemical group C.C=C XTEXMYNJEMCTNI-UHFFFAOYSA-N 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000004200 deflagration Methods 0.000 description 2
- 239000002737 fuel gas Substances 0.000 description 2
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/10—Nitrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/108—Hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7022—Aliphatic hydrocarbons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7022—Aliphatic hydrocarbons
- B01D2257/7025—Methane
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0225—Other waste gases from chemical or biological warfare
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/20—Capture or disposal of greenhouse gases of methane
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention belongs to the technical field of recycling of flare gas discharged from a polyethylene device, and particularly relates to a method for recycling nitrogen in the flare gas discharged from the polyethylene device, which is characterized by comprising the following steps of: after passing through a flare gas compressor, a catalytic dehydrogenation unit and a pressure swing adsorption separation unit in sequence, the hydrocarbon components are adsorbed, nitrogen enters a nitrogen pipe network of a degassing bin of the device, and desorption gas containing hydrocarbon components such as methane and ethane is sent to a flare. According to the invention, the nitrogen with the purity of more than 99.9% is obtained, so that the nitrogen can directly enter a nitrogen pipe network of a degassing bin of the device; and simultaneously, the hydrocarbon-rich gas with the heat value increased is obtained.
Description
Technical Field
The invention belongs to the technical field of recycling polyethylene device flare gas, and particularly relates to a method for recycling nitrogen in polyethylene device flare gas.
Background
Different production processes are adopted for the polyethylene device, the purity requirements of the degassing bin on nitrogen are different, and the purity of nitrogen is required to be more than 98% in some production processes; some production processes require more than 99.9%.
In the production process of polyethylene, a large amount of tail gas containing hydrocarbon components such as methane, ethylene, ethane, hydrogen, nitrogen, butene, pentane and the like is discharged in a reactor and a degassing bin, most hydrocarbon components such as butene, pentane and the like are recovered by the tail gas through a low-pressure and high-pressure condensation process, part of ethylene and ethane are recovered through membrane separation, and the rest gas is burnt out as flare gas. The methane ethylene and other gases in the tail gas belong to the components which are not easy to compress, the nitrogen belongs to the inorganic matters, the recovery effect of the methane ethylene and the nitrogen is limited, meanwhile, the recovery device investment and the applicability are limited, C4 and C5 are condensed and recovered through a membrane, the residual content of butene-1 and isopentane is low, and the methane ethylene and the residual content can only be used as fuel gas and can be burnt in a torch system. The hydrocarbon components are needed to be separated from the polyethylene powder of the reactor, no consumption link exists, and the hydrocarbon components can accumulate in the recycling process of nitrogen to influence the degassing effect.
The volume fraction of the flare gas is more than 90% and is nitrogen, the heat value is low, and the high heat value fuel gas needs to be supplemented to the flare pipe network to ensure the normal combustion of the flare. And the flare is emptied, so that not only is energy wasted, but also a certain light, heat, noise and other environmental influences and pollution are caused. How to recycle nitrogen in the flare gas, and the nitrogen pipe network is input into a degassing bin of the device after the purity reaches 99.9%, and the value of the flare gas is improved at the same time, is the development direction.
Chinese patent ZL200910038599.7, "method for completely recycling polyethylene device tail gas", discloses a method for recycling polyethylene tail gas by combining pressure condensation, membrane separation and pressure swing adsorption, but only can make H 2 +N 2 Up to 99% of the purity, of which 1% is also the hydrocarbon component of methane and ethylene; chinese patent ZL201510475706.8, "a method and apparatus for recovering hydrocarbon component and nitrogen from polyethylene tail gas", discloses a method for recovering polyethylene tail gas by combining pressure condensation, catalytic dehydrogenation and pressure swing adsorption, and also can only make H 2 +N 2 And up to 99% of the purity of (c) and 1% of hydrocarbon components such as methane and ethylene.
The method has a certain effect, but the removal precision of hydrocarbon components such as methane, ethane and the like is limited, the purity of nitrogen cannot reach a level of more than 99.9 percent, and 1 percent of the components such as methane, ethane, ethylene and the like are contained in the nitrogen, and the purity requirements of nitrogen for a degassing bin are different due to different production processes adopted by the polyethylene device, so that the nitrogen with the purity of 99 percent cannot meet the use requirements of the degassing bins of all the polyethylene devices at present. The polyethylene device is provided with the exhaust gas of the reactor, the exhaust gas of the degassing bin and the like, and for the exhaust gas of the reactor, the concentration of C4, C5 and other components is higher, so that the C4 and C5 in the exhaust gas can be recovered by a condensation procedure; for the exhaust gas of the degassing bin, the nitrogen concentration is higher (more than 90 percent and even up to 98.5 percent), the concentration of components above C4 is low, the partial pressure is low, and the common condensing method adopting the polyethylene device has an unsatisfactory effect.
The removal of hydrocarbon components from the nitrogen as much as possible, the purity of which reaches the level of the nitrogen line that can be fed to the degassing compartment of the polyethylene plant, is currently desired.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for recycling nitrogen in flare gas of a polyethylene device, which comprises the steps of coupling catalytic dehydrogenation, membrane separation and pressure swing adsorption to obtain product nitrogen with purity of more than 99.9%; the permeation gas of the membrane separation unit is mixed with the desorption gas of the pressure swing adsorption unit, so that the heat value is improved, and a fire removing torch pipe network is provided.
The method for recycling nitrogen in the flare gas of the polyethylene device, which solves the technical problems, comprises raw material gas and is characterized in that: after passing through a flare gas compressor, a catalytic dehydrogenation unit and a pressure swing adsorption separation unit in sequence, hydrocarbon components are adsorbed, nitrogen enters a nitrogen pipe network of a degassing bin of the device, and membrane permeation gas containing hydrocarbon components such as methane and ethane and desorption gas subjected to pressure swing adsorption are removed from a flare.
The compressor is pressurized, the catalytic dehydrogenation unit removes hydrogen in the flare gas, the membrane separation unit separates and removes partial hydrocarbon components, and the residual gas after permeation enters the pressure swing adsorption separation unit for continuous separation. When the polyethylene tail gas passes through the membrane in the membrane separation unit, most of hydrogen and nitrogen are on one side, and most of hydrocarbon such as methane and ethane and a small amount of hydrogen and nitrogen are on the other side, dehydrogenation is placed in front of the membrane, so that sufficient reaction of ethylene and hydrogen is ensured, and dehydrogenation precision is ensured.
Polyethylene tail gas has a hydrogen component that is removed by catalytic dehydrogenation, whereas membrane separation and PSA alone do not allow low cost separation of hydrogen from nitrogen, not to mention achieving a purity of 99.9% for nitrogen.
The raw material gas is flare gas discharged to a flare by a polyethylene device, and the pressure is 4-10 KPag.
A compressor in the compressor unit pressurizes the polyethylene device flare gas to 0.4-0.6 MPag.
The reaction temperature of the reactor of the dehydrogenation unit is 70-200 ℃; the temperature is gradually increased along with the activity attenuation of the catalyst at the initial stage, the middle stage and the final stage of the use, so that the hydrogen removal precision can be ensured. The dehydrogenation catalyst is a metal catalyst.
The pressure swing adsorption unit comprises N adsorbers, a series of program control valves, pipelines, a pressure gauge, a vacuum pump and other devices, wherein each device forms a continuous operation system by pipelines, the devices are connected with each other to form a continuous operation system, and methane and other hydrocarbon components in the flare gas of the polyethylene device are adsorbed to obtain high-purity nitrogen.
The N is more than or equal to 4.
Each adsorber is subjected to the adsorption, pressure equalization drop, reverse discharge, evacuation flush, pressure equalization rise and final pressure rise operating steps in sequence in one cycle.
The adsorber is filled with adsorbents in layers, and 4 adsorbents of alumina, modified silica gel, modified activated carbon and modified molecular sieve are sequentially filled from bottom to top, wherein the dosage proportion of the adsorbents is changed along with the different composition contents of polyethylene tail gas.
The method also comprises a membrane separation unit which is arranged between the catalytic dehydrogenation unit and the pressure swing adsorption separation unit. Is suitable for the condition of low nitrogen amount. The membrane separation unit adopts an organic membrane to separate nitrogen and hydrocarbon components, and more than 65% of hydrocarbon components in the flare gas are removed.
The method comprises the following specific steps:
(1) Pressurizing: the polyethylene device discharges flare gas and is pressurized to 0.4 to 0.6MPag through a compressor;
(2) Catalytic dehydrogenation: the pressurized flare gas enters a catalytic dehydrogenation reactor, and hydrogen reacts with ethylene to generate ethane at the reaction temperature of 70-200 ℃ so as to achieve the purpose of removing hydrogen.
(3) Purifying nitrogen by the pressure swing adsorption separation unit: the gas after catalytic dehydrogenation enters a pressure swing adsorption separation unit, and hydrocarbon components such as methane, ethylene, ethane and the like are adsorbed by 4 adsorbents filled in an adsorption tower in the pressure swing adsorption separation unit.
Nitrogen with a purity of 99.9% was obtained from the outlet of the top of the adsorption column, and was sent to the nitrogen line network of the degasification silo of the apparatus. And (5) removing the desorption gas containing methane and ethane obtained during desorption of the pressure swing adsorption unit to a torch.
When a membrane separation unit is provided, the specific steps of the method of the invention are as follows:
(1) Pressurizing: the polyethylene device discharges flare gas and is pressurized to 0.4 to 0.6MPag through a compressor;
(2) Catalytic dehydrogenation: the pressurized flare gas enters a catalytic dehydrogenation reactor, and hydrogen reacts with ethylene to generate ethane at the reaction temperature of 70-200 ℃ so as to achieve the purpose of removing hydrogen.
(3) Membrane separation of part of hydrocarbons: the membrane unit comprises more than 1 membrane component, namely more than 1 membrane separation component is connected in series or in parallel for separation. When the flare gas passes through the organic membrane, hydrocarbon components such as ethane, ethylene, C4 and the like preferentially permeate compared with nitrogen, methane and the like by utilizing the difference of the dissolution and diffusion properties of different gas molecules in the membrane under the action of permeation driving force, so that the purpose of separation is achieved. Permeate gas of the membrane unit is discharged out of the pipe network of the fire removing torch through a pipeline; the residual gas enters the pressure swing adsorption separation unit through a pipeline.
(4) Purifying nitrogen by the pressure swing adsorption separation unit: the residual gas after membrane separation enters a pressure swing adsorption separation unit, and hydrocarbon components such as methane, ethylene, ethane and the like are adsorbed by 4 adsorbents filled in an adsorption tower in the pressure swing adsorption separation unit.
Each adsorber of the pressure swing adsorption unit is subjected to the same steps, and each adsorber is sequentially subjected to the steps of adsorption, pressure equalization drop, reverse discharge, evacuation and flushing, pressure equalization rise and final pressure rise. Taking an adsorber as an example, the specific steps are as follows:
(A) Adsorption of
The residual gas after separation by the membrane separation unit is sent into an absorber from bottom to top through a pipeline and a program control valve for absorption, the absorber in the absorber absorbs components such as methane, ethane, ethylene and the like in the raw material gas, and the nitrogen which is not absorbed is discharged from the top of the absorber. When the content of methane, ethane and other components at the outlet of the adsorber reaches 0.1%, the program control valve for the raw material to enter is closed, the raw material gas is stopped from entering the adsorber, and the adsorption is stopped.
(B) Pressure equalization drop
And opening the pressure equalization drop program control valve to enable the gas in the adsorber which completes the adsorption step to enter the adsorber which just completes the evacuation step through the pressure equalization drop program control valve along the adsorption direction until the pressures of 2 adsorbers are consistent, thus reducing the pressure in the adsorbers and desorbing partial components such as methane, ethane, ethylene and the like.
(3) Reverse-playing
After the pressure equalization drop step is completed, the program control valve is opened, the gas in the adsorber is discharged out of the adsorber against the adsorption direction, the adsorbent continues to desorb, and the pressure of the adsorber is reduced to approximately 0.02MPag.
(4) Evacuation and flushing
The pressure of the adsorption bed layer is further reduced by utilizing a vacuum pump to approach the normal pressure, and the adsorption bed layer is pumped out and flushed at the same time, so that components such as methane, ethane, ethylene and the like are desorbed and flow out of the adsorption bed layer, the adsorbent can be thoroughly desorbed, and the purity of the nitrogen product is ensured.
(5) Pressure equalization rise
The nitrogen flowing out from the top of the absorber in the pressure equalization drop step is used for boosting the absorber which completes the evacuation step until the pressure of the two absorption towers is consistent.
(6) Final boost pressure
After the pressure equalization rising step is completed, the product nitrogen is used for rising the pressure of the adsorber, the pressure is raised to be close to the adsorption pressure, and the next adsorption is prepared.
Each adsorber will undergo the same steps, staggered in time sequence, to ensure that the separation process proceeds continuously.
According to the invention, after the polyethylene device discharged flare gas passes through the compression unit, the dehydrogenation unit, the membrane separation unit and the pressure swing adsorption separation unit, nitrogen with purity of more than 99.9% can be obtained, and the nitrogen can be directly fed into a nitrogen pipe network of a degassing bin of the device; the resources are saved, and the pollution is reduced; and simultaneously, the hydrocarbon-rich gas with the heat value increased is obtained. The hydrocarbon-rich gas is permeation gas of the membrane unit and desorption gas of the pressure swing adsorption unit, and contains hydrocarbon components such as methane, ethylene, ethane and the like, and is a fire removing torch. After the treatment by the method, the gas heat value of the discharging flare pipe network is improved by more than 4 times. Is especially suitable for recycling nitrogen in the tail gas of a degassing bin of a polyethylene device.
Drawings
FIG. 1 is a schematic flow chart of a device in accordance with embodiment 2 of the present invention
FIG. 2 is a schematic flow chart of a device according to embodiment 3 of the present invention
FIG. 3 is a schematic flow chart of a device in accordance with embodiment 4 of the present invention
FIG. 4 is a schematic structural view of a dehydrogenation unit according to the present invention
Wherein, the mark in the figure is: 1. feed gas inlet pipe 2, dehydrogenation unit 3, compressor 4, pipeline 5, adsorber 6, programmable valve 7, heat insulating layer 8, regulating valve 9, nitrogen outlet pipe 10, desorption gas outlet pipe 11, vacuum pump 12, pressure gauge 13, membrane separation unit 14, permeation pipeline 15, dehydrogenation heater 16, reactor 17, cooler
Detailed Description
The invention will be described in further detail with reference to the accompanying drawings and detailed description, wherein the compressors, dehydrogenation reactors, adsorbers, membrane units and membrane modules used are conventional:
example 1
In the method for recycling nitrogen in the flare gas of the polyethylene device, the raw material gas is the flare gas discharged to the flare of the polyethylene device, and the pressure is 10KPag; after the raw material gas sequentially passes through a flare gas compressor, a catalytic dehydrogenation unit and a pressure swing adsorption separation unit through a raw material gas input pipe, hydrocarbon components are adsorbed, nitrogen enters a nitrogen pipe network of a degassing bin of the device through a nitrogen output pipe, and desorption gas containing hydrocarbon components such as methane and ethane is sent to a flare through a desorption gas output pipe. The compressor in the compressor unit pressurizes the polyethylene device flare gas to 0.5MPag. The reaction temperature of the reactor of the dehydrogenation unit is 70-200 ℃. The dehydrogenation catalyst is a metal catalyst.
The method comprises the following specific steps:
(1) Pressurizing: the polyethylene device discharges flare gas and is pressurized to 0.4 to 0.6MPag through a compressor;
(2) Catalytic dehydrogenation: the pressurized flare gas enters a catalytic dehydrogenation reactor, and hydrogen reacts with ethylene to generate ethane at the reaction temperature of 70-200 ℃ so as to achieve the purpose of removing hydrogen.
(3) Purifying nitrogen by the pressure swing adsorption separation unit: the gas after catalytic dehydrogenation enters a pressure swing adsorption separation unit, and hydrocarbon components such as methane, ethylene, ethane and the like are adsorbed by 4 adsorbents filled in an adsorption tower in the pressure swing adsorption separation unit.
And obtaining nitrogen with purity equal to or higher than 99.9% from the outlet of the top of the adsorption tower, and removing the nitrogen pipe network. And (5) sending the desorption gas containing ethane and ethylene obtained during desorption of the pressure swing adsorption unit to a torch.
The pressure swing adsorption unit comprises 4 or more adsorbers, a series of program control valves, pipelines, pressure gauges, vacuum pumps and other devices, and is connected by pipelines to form a continuous operation system, wherein the outer surfaces of the adsorbers are provided with heat insulation layers, and methane and other hydrocarbon components in the flare gas of the polyethylene device are adsorbed to obtain high-purity nitrogen.
The inside of the absorber is filled with the adsorbent in layers, 4 adsorbents of alumina, modified silica gel, modified activated carbon and modified molecular sieve are sequentially filled from bottom to top, and the dosage proportion of the adsorbent is changed along with the different composition contents of the polyethylene tail gas.
Each adsorber is cycled through adsorption, pressure equalization drop, reverse discharge, evacuation flush, pressure equalization rise, and final pressure boost operating steps in sequence. The process gas discharged from the absorber in the pressure equalization step is sent to the absorber in the pressure equalization step. The particle size of the adsorbent is as follows: 3-5 mm of alumina, 1-4 mm of modified activated carbon, 1-5 mm of modified silica gel and 1-5 mm of modified molecular sieve.
The specific steps of the adsorber A are as follows:
(1) Adsorption of
The flare gas after dehydrogenation by the catalytic dehydrogenation unit is sent into an absorber from bottom to top through a pipeline and a program control valve to be absorbed, 4 adsorbents filled in the absorber adsorb components such as methane and ethane in the raw material gas, and the nitrogen which is not adsorbed is discharged from the top of the absorber. When the components of methane, ethane and the like at the outlet of the adsorber reach 0.1%, the program control valve for the raw material to enter is closed, the raw material gas is stopped from entering the adsorber, and the adsorption is stopped.
(2) Pressure equalization drop
And opening the pressure equalization drop program control valve to enable the gas in the adsorber which completes the adsorption step to enter the adsorber which just completes the evacuation step through the pressure equalization drop program control valve along the adsorption direction until the pressures of 2 adsorbers are consistent, thus reducing the pressure in the adsorbers which complete the adsorption and desorbing partial components such as methane, ethane, ethylene and the like.
(3) Reverse-playing
After the pressure equalization drop step is completed, the program control valve is opened, the gas in the adsorber is discharged out of the adsorber against the adsorption direction, the adsorbent continues to desorb, and the pressure of the adsorber is reduced to approximately 0.02MPag.
(4) Evacuation flushing
The pressure of the adsorption bed layer is further reduced by using a vacuum pump to the adsorption device close to normal pressure, and the adsorption device is flushed while being evacuated, so that components such as methane, ethane, ethylene and the like are desorbed and flow out of the adsorption device, and the adsorbent is regenerated.
(5) Pressure equalization rise
The nitrogen flowing out from the top of the absorber in the pressure equalization drop step is used for boosting the absorber which completes the evacuation step until the pressure of the two absorption towers is consistent.
(6) Final boost pressure
After the pressure equalization rising step is completed, the product nitrogen is used for rising the pressure of the adsorber, the pressure is raised to be close to the adsorption pressure, and the next adsorption is prepared. Each adsorber will undergo the same steps, staggered in time sequence, to ensure that the separation process proceeds continuously.
The device system comprises a flare gas input pipe, a compressor, a desorption gas output pipe, a flare pipe network and a nitrogen output pipe, wherein the flare gas input pipe is connected with the compressor, a dehydrogenation unit and a pressure swing adsorption separation unit are also arranged, and the compressor is connected with the dehydrogenation unit; the dehydrogenation unit is connected with the pressure swing adsorption separation unit, the top end of the pressure swing adsorption separation unit is connected with the nitrogen output pipe, the bottom end of the pressure swing adsorption separation unit is connected with the desorption gas output pipe, and the desorption gas output pipe is connected with the flare pipe network. The dehydrogenation unit comprises a dehydrogenation reactor, a cooler and a heater, wherein the heater is connected with the dehydrogenation reactor, and the dehydrogenation reactor is connected with the cooler. The dehydrogenation reactor is internally provided with a catalyst, the components in the flare gas react under the action of the catalyst to remove hydrogen, and the operation temperature of the dehydrogenation unit is 70-200 ℃. The flare gas is heated before entering the dehydrogenation reactor, and enters a cooler for cooling after dehydrogenation reaction, and then enters the next unit.
The pressure swing adsorption unit comprises a pipeline, N adsorbers, a pressure gauge, a program control valve and a vacuum pump, wherein the adsorbers are connected in parallel; the upper end and the lower end of each adsorber are respectively provided with a program control valve, and a nitrogen output pipe is connected with the top end of each adsorber through the program control valves; one end of the vacuum pump is connected with the bottom end of the absorber through a program control valve, and the other end of the vacuum pump is connected with a desorption gas output pipe; the pressure gauge is arranged between the top end of the absorber and the program control valve. N is more than or equal to 4. And a regulating valve is arranged between the program control valve and the nitrogen output pipe.
Example 2
In the method for recycling nitrogen in the flare gas of the polyethylene device, the raw material gas is the flare gas discharged to the flare of the polyethylene device, and the pressure is 6KPag; the raw material gas sequentially passes through a flare gas compressor, a catalytic dehydrogenation unit, a membrane separation unit and a pressure swing adsorption separation unit through a raw material gas input pipe, hydrocarbon components are adsorbed, nitrogen enters a nitrogen pipe network of the polyethylene device through a nitrogen output pipe, and desorption gas containing hydrocarbon components such as methane and ethane is discharged to a flare through a desorption gas output pipe. Wherein, the compressor is pressurized, the catalytic dehydrogenation unit removes hydrogen in the flare gas, the membrane separation unit separates and removes partial hydrocarbon components, and the residual gas after permeation enters the pressure swing adsorption separation unit for continuous separation. The compressor in the compressor unit pressurizes the polyethylene device flare gas to 0.6MPag. The reaction temperature of the reactor of the dehydrogenation unit is 70-200 ℃. The dehydrogenation catalyst is a metal catalyst.
The method comprises the following specific steps:
(1) Pressurizing: the polyethylene device discharges flare gas and is pressurized to 0.4 to 0.6MPag through a compressor;
(2) Catalytic dehydrogenation: the pressurized flare gas enters a catalytic dehydrogenation reactor, and hydrogen reacts with ethylene to generate ethane at the reaction temperature of 70-200 ℃ so as to achieve the purpose of removing hydrogen.
(3) Membrane separation of part of hydrocarbons: the membrane unit comprises more than 1 membrane component, and more than 1 membrane component is connected in series or in parallel. When the flare gas passes through the organic membrane, hydrocarbon components such as ethane, ethylene, C4 and the like preferentially permeate compared with nitrogen, methane and the like by utilizing the difference of the dissolution and diffusion properties of different gas molecules in the membrane under the action of permeation driving force, so that the purpose of separation is achieved. Permeate gas of the membrane unit is discharged out of the pipe network of the fire removing torch through a pipeline; the residual gas enters the pressure swing adsorption separation unit through a pipeline. Most of hydrocarbon is separated from the permeated gas, the permeated gas has high heat value, and the permeated gas can be directly burnt by a fire-removing torch pipe network.
(4) Purifying nitrogen by the pressure swing adsorption separation unit: the residual gas after membrane separation enters a pressure swing adsorption separation unit, and hydrocarbon components such as methane, ethylene, ethane and the like are adsorbed by 4 adsorbents filled in an adsorption tower in the pressure swing adsorption separation unit.
And obtaining nitrogen with purity of more than 99.9% from the outlet of the top of the adsorption tower, and removing the nitrogen pipe network of the degassing bin of the polyethylene device. And (3) removing the desorption gas containing hydrocarbon components such as methane and ethane obtained during desorption by the pressure swing adsorption unit to a torch.
The pressure swing adsorption unit comprises 4 or more adsorbers, a series of program control valves, pipelines, pressure gauges, vacuum pumps and other devices, and is connected by pipelines to form a continuous operation system, wherein the outer surfaces of the adsorbers are provided with heat insulation layers, and methane and other hydrocarbon components in the flare gas of the polyethylene device are adsorbed to obtain high-purity nitrogen.
The inside of the absorber is filled with the adsorbent in layers, 4 adsorbents of alumina, modified silica gel, modified activated carbon and modified molecular sieve are sequentially filled from bottom to top, and the dosage proportion of the adsorbent is changed along with the different composition contents of the polyethylene tail gas.
Each adsorber is cycled through adsorption, pressure equalization drop, reverse discharge, evacuation flush, pressure equalization rise, and final pressure boost operating steps in sequence. The process gas discharged from the absorber in the pressure equalization step is sent to the absorber in the pressure equalization step. The specific procedure was as in example 1.
The device system for recycling nitrogen in the polyethylene device flare gas is provided with a flare gas input pipe, a compressor, a dehydrogenation unit, a membrane separation unit, a permeation pipeline, a pressure swing adsorption separation unit, a desorption gas output pipe, a flare pipe network and a nitrogen output pipe, wherein the flare gas input pipe is connected with the compressor, and the compressor is connected with the dehydrogenation unit; the dehydrogenation unit is connected with the pressure swing adsorption separation unit, the top end of the pressure swing adsorption separation unit is connected with the nitrogen output pipe, the bottom end of the pressure swing adsorption separation unit is connected with the desorption gas output pipe, and the desorption gas output pipe is connected with the flare pipe network; the membrane separation unit comprises 1 or more membrane pieces, and the dehydrogenation unit is connected with the membrane separation unit; the residual gas seeped in the membrane separation unit enters the pressure swing adsorption separation unit through a pipeline; the membrane separation unit is connected with the flare pipe network through a permeation pipeline, so that permeation gas of the membrane unit is discharged out of the flare pipe network. The above units are connected to each other by pipes. The membrane separation unit comprises 1 or more membrane pieces, namely, more than 1 membrane pieces are connected in series or in parallel. The membrane separation unit adopts 1 or more organic membrane parts to separate nitrogen and hydrocarbon components, and removes more than 65% of hydrocarbon components in the flare gas.
The dehydrogenation unit comprises a dehydrogenation reactor, a cooler and a heater, wherein the heater is connected with the dehydrogenation reactor, and the dehydrogenation reactor is connected with the cooler. The dehydrogenation reactor is internally provided with a catalyst, the components in the flare gas react under the action of the catalyst to remove hydrogen, and the operation temperature of the dehydrogenation unit is 70-200 ℃. The flare gas is heated before entering the dehydrogenation reactor, and enters a cooler for cooling after dehydrogenation reaction, and then enters the next unit.
Example 3
Other things as in example 1, a polyethylene unit discharged 1000Nm of flare gas 3 And/h, the composition is shown in Table 1:
table 1 polyethylene device flare gas discharge
| Component (A) | H 2 | N 2 | CH 4 | C 2 H 6 | C 2 H 4 | C 4 | C 5 + | H 2 O |
| Content, v% | 0.03 | 98.37 | 0.03 | 0.1 | 0.37 | 0.23 | 0.07 | 0.80 |
Pressure 4KPag, total 1000Nm 3 The polyethylene device of/h discharges the flare gas to be pressurized to 0.4MPag through a compressor, and enters a dehydrogenation unit, the reaction temperature of a reactor in the dehydrogenation unit is 70-200 ℃ after the reaction of hydrogen and ethylene to generate ethane. The flare gas from which hydrogen is removed enters a pressure swing adsorption unit which consists of 4 adsorbers, a series of program control valves, regulating valves, a vacuum pump and other devices, wherein the adsorbers are provided with heat insulation layers, and the devices are connected through pipelines. The adsorbent in the adsorber adsorbs methane, ethane, ethylene, C4 and C5 + The components, the nitrogen which is not adsorbed, are discharged from the top of the absorber through a pipeline to obtain nitrogen with purity of more than 99.9 percent, and the nitrogen enters a nitrogen pipe network of a degassing bin of the polyethylene device. Because the feedstock hydrocarbon component content in the examples is not high, membrane units may not be required for separation. After treatment, the gas heat value of the flare discharging pipe network is improved by more than 4 times.
Each adsorber is subjected to the steps of adsorption, pressure equalization drop, reverse discharge, evacuation flushing, pressure equalization rise, final pressure rise, and the like in sequence.
Example 4
Other things as in example 1, a polyethylene unit discharged 3000Nm of flare gas 3 And/h, composition shown in Table 2:
table 2 polyethylene device flare gas discharge
| Component (A) | H 2 | N 2 | CH 4 | C 2 H 6 | C 2 H 4 | C 4 | C 5 + | H 2 O |
| Content, v% | 0.1 | 94.82 | 0.1 | 1.0 | 2.5 | 0.5 | 0.16 | 0.82 |
Pressure 6KPag, total 2000Nm 3 The polyethylene device of/h discharges the flare gas to be pressurized to 0.5MPag through a compressor, and enters a dehydrogenation unit, the reaction temperature of a reactor in the dehydrogenation unit is 70-200 ℃ after the reaction of hydrogen and ethylene to generate ethane. The flare gas with hydrogen removed enters a membrane separation unit for separation, 65% of hydrocarbon components in the flare gas are removed through membrane permeation, the residual gas after permeation enters a pressure swing adsorption unit consisting of 5 adsorbers, a series of program control valves and other devices, and 4 adsorbents filled in the adsorbers adsorb methane, ethane, ethylene, C4 and C5 in the residual gas + The components, the nitrogen which is not adsorbed, are discharged from the top of the absorber through a pipeline to obtain nitrogen with the purity of more than 99.9 percent, and the nitrogen enters a nitrogen pipe network of a degassing bin of the polyethylene device. Hydrocarbon-rich gas deflagration torch pipe network of membrane separation unit and PSA unit. After treatment, the gas heat value of the flare discharging pipe network is improved by more than 4 times.
In the example, 5 adsorbers are sequentially subjected to the steps of adsorption, pressure equalization drop, reverse discharge, evacuation flushing, pressure equalization rise, final pressure rise and the like.
Example 5
Other things as in example 1, a polyethylene unit discharged 3000Nm of flare gas 3 And/h, composition shown in Table 3:
table 3 polyethylene device flare gas discharge
| Component (A) | H 2 | N 2 | CH 4 | C 2 H 6 | C 2 H 4 | C 4 | C 5 + | H 2 O |
| Content, v% | 0.2 | 96.18 | 0.08 | 0.7 | 1.6 | 0.3 | 0.12 | 0.82 |
Pressure 6KPag, total 3000Nm 3 The polyethylene device of/h discharges the flare gas to be pressurized to 0.6MPag by a compressor, and enters a dehydrogenation unit, wherein the reaction temperature of a reactor in the dehydrogenation unit is 70-200 ℃. The hydrogen reacts with ethylene to generate ethane, the flare gas with the hydrogen removed enters a membrane separation unit for separation, 65 percent of hydrocarbon components in the flare gas are removed through membrane permeation gas, the residual gas enters a pressure swing adsorption unit which consists of 6 adsorbers, a series of program control valves and other devices, and 4 adsorbents filled in the adsorbers adsorb methane, ethane, ethylene, C4 and C5 in the hydrogen and ethylene + The components, the nitrogen which is not adsorbed is discharged from the top of the absorber through a pipeline to obtain the nitrogen with the purity of more than 99.9 percent, and the nitrogen enters the polyethyleneNitrogen line network for degassing bins of alkene plants. Hydrocarbon-rich gas deflagration torch pipe network of membrane separation unit and PSA unit. After treatment, the gas heat value of the flare discharging pipe network is improved by more than 4 times.
In the example, 6 adsorbers are sequentially subjected to the steps of adsorption, pressure equalization drop, reverse discharge, evacuation flushing, pressure equalization rise, final pressure rise and the like.
If the nitrogen with the purity of more than 99.9 is needed to be obtained from the exhaust gas of the degassing bin, when the content of hydrocarbon components in the exhaust gas is higher, for example, more than 2 percent, the effect can not be achieved by only adopting one section of PSA recovery, and the 2 sections of PSA flow path is long; while nitrogen alone does not reach 99.9% purity by touch separation, the use of membrane+psa is the most suitable method with 2 technical advantages, and is also the best combination from the standpoint of footprint, and is also readily accepted for industrialization.
In the invention, a catalytic process is updated, and the catalytic reaction temperature is 70-200 ℃; when the content of hydrocarbon components in the exhaust gas is higher, a membrane separation unit is added, so that the process flow is simple; the process of the pressure swing adsorption unit is updated, 4 kinds of adsorbents are needed, the filling sequence of the adsorbents and the adsorption process steps are needed, the final effect of adsorption separation is achieved on the whole, and the purity of nitrogen reaches 99.9% or more.
While the basic principles and main features of the present invention and advantages thereof have been shown and described, the foregoing embodiments and description are merely illustrative of the principles of the present invention, and various changes and modifications can be made therein without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A method for recycling nitrogen in flare gas of a polyethylene device comprises raw material gas, and is characterized in that the raw material gas sequentially passes through a flare gas compressor, a catalytic dehydrogenation unit, a membrane separation unit and a pressure swing adsorption separation unit, hydrocarbon components are adsorbed, nitrogen enters a nitrogen pipe network of a degassing bin of the device, and desorption gas of hydrocarbon components containing methane and ethane is removed from the flare;
the method comprises the following specific steps:
(1) Pressurizing: pressurizing the polyethylene device discharged flare gas to 0.4-0.6 MPag through a compressor;
(2) Catalytic dehydrogenation: the pressurized flare gas enters a catalytic dehydrogenation reactor, and hydrogen reacts with ethylene to generate ethane at the reaction temperature of 70-200 ℃ so as to achieve the purpose of removing hydrogen;
(3) Membrane separation of part of hydrocarbons: the membrane unit comprises more than 1 membrane component, namely more than 1 membrane separation component is connected in series or in parallel for separation; when flare gas passes through the organic membrane, ethane, ethylene and C4 components preferentially permeate nitrogen and methane by utilizing the difference of dissolution and diffusion properties of different gas molecules in the membrane under the action of permeation driving force, so that the purpose of separation is achieved; permeate gas of the membrane unit is discharged out of the pipe network of the fire removing torch through a pipeline; the residual gas enters a pressure swing adsorption separation unit through a pipeline;
(4) Purifying nitrogen by the pressure swing adsorption separation unit: the residual gas after membrane separation enters a pressure swing adsorption separation unit, and in the pressure swing adsorption separation unit, the components of methane, ethylene and ethane are adsorbed by 4 adsorbents filled in an adsorption tower; nitrogen with a purity of more than 99.9% is obtained.
2. The method of recovering nitrogen from polyethylene plant flare gas of claim 1, wherein: the raw material gas is flare gas discharged to a flare by a polyethylene device, and the pressure is 4-10 KPag.
3. The method of recovering nitrogen from polyethylene plant flare gas of claim 1 or 2, characterized by: the compressor pressurizes the polyethylene device flare gas to 0.4-0.6 MPag.
4. The method of recovering nitrogen from polyethylene plant flare gas of claim 1, wherein: the reaction temperature of the reactor of the catalytic dehydrogenation unit is 70-200 ℃.
5. The method of recovering nitrogen from polyethylene plant flare gas of claim 1, wherein: the pressure swing adsorption separation unit comprises N adsorbers, a program control valve, a pipeline and a vacuum pump, wherein various equipment forms a continuous operation system by pipelines, and methane and other hydrocarbon components in the flare gas of the polyethylene device are adsorbed to obtain high-purity nitrogen.
6. The method of recovering nitrogen from polyethylene plant flare gas of claim 5, wherein: n is more than or equal to 4.
7. The method of recovering nitrogen from polyethylene plant flare gas of claim 5, wherein: each adsorber cycle is subjected to adsorption, pressure equalization down, reverse blow, evacuation flush, pressure equalization up, and final pressure boost operating steps in sequence.
8. The method of recovering nitrogen from polyethylene plant flare gas of claim 5, wherein: the adsorber is filled with adsorbents in layers, and 4 adsorbents of alumina, modified silica gel, modified activated carbon and modified molecular sieve are sequentially filled from bottom to top, wherein the dosage proportion of the adsorbents is changed along with the different composition contents of polyethylene tail gas.
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