CN106861452A - Membrane module, the hydrogen gas recovering device based on membrane module and Hydrogen Separation method - Google Patents
Membrane module, the hydrogen gas recovering device based on membrane module and Hydrogen Separation method Download PDFInfo
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- CN106861452A CN106861452A CN201710118744.7A CN201710118744A CN106861452A CN 106861452 A CN106861452 A CN 106861452A CN 201710118744 A CN201710118744 A CN 201710118744A CN 106861452 A CN106861452 A CN 106861452A
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- 239000012528 membrane Substances 0.000 title claims abstract description 182
- 239000001257 hydrogen Substances 0.000 title claims abstract description 63
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 63
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000926 separation method Methods 0.000 title claims abstract description 25
- 150000002431 hydrogen Chemical class 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 74
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 70
- 239000002808 molecular sieve Substances 0.000 claims abstract description 64
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000919 ceramic Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 230000001105 regulatory effect Effects 0.000 claims abstract description 19
- 238000007747 plating Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000004064 recycling Methods 0.000 claims abstract description 11
- 230000006641 stabilisation Effects 0.000 claims abstract description 6
- 238000011105 stabilization Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims description 12
- 230000007704 transition Effects 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000010425 asbestos Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 229910052895 riebeckite Inorganic materials 0.000 claims description 4
- 239000005060 rubber Substances 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- -1 carclazyte Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004014 plasticizer Substances 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000000565 sealant Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims 1
- 239000010408 film Substances 0.000 description 37
- 238000000034 method Methods 0.000 description 16
- 230000008569 process Effects 0.000 description 9
- 230000035699 permeability Effects 0.000 description 7
- 238000011084 recovery Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
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- 238000004806 packaging method and process Methods 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 2
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 229920001220 nitrocellulos Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000005713 exacerbation Effects 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
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- 239000004088 foaming agent Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
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- 238000006317 isomerization reaction Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
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- 239000011148 porous material Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
-
- 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
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/06—Tubular membrane modules
-
- 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
- B01D2053/221—Devices
-
- 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
- B01D2317/00—Membrane module arrangements within a plant or an apparatus
- B01D2317/04—Elements in parallel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2317/00—Membrane module arrangements within a plant or an apparatus
- B01D2317/06—Use of membrane modules of the same kind
Abstract
The invention provides a kind of membrane module, the hydrogen gas recovering device based on membrane module and Hydrogen Separation method, the membrane module includes multiple Carbon Molecular Sieve Membranes, and each Carbon Molecular Sieve Membrane ties up to form membrane module into tubulose, and many Carbon Molecular Sieve Membranes；Carbon Molecular Sieve Membrane includes ceramic membrane and is plated in the film plating layer on its surface, and the film plating layer of each Carbon Molecular Sieve Membrane is exposed at outer surface；The hydrogen gas recovering device includes raw material gas tank, temperature control device and membrane module, and three is connected by the first pipeline, and membrane module is connected with tail gas recycle tank and hydrogen recycling can；The Hydrogen Separation method is comprised the following steps：The regulating valve on the first pipeline is opened, unstripped gas is delivered to the first pipeline by the regulating valve closed on the second pipeline；Adjustment temperature control device, by unstripped gas temperature stabilization after, be delivered to membrane module；After unstripped gas carries out Hydrogen Separation through membrane module, hydrogen is reclaimed by hydrogen recycling can, and tail gas is reclaimed by tail gas recycle tank.The present invention can reduce the volume of membrane module, save materials.
Description
Technical field
The invention belongs to inorganic technical field of membrane separation, in particular to a kind of membrane module, the hydrogen based on membrane module
Retracting device and Hydrogen Separation method.
Background technology
During some extensive process (as reformed and cracking) of modern petrochemical and petroleum refining industry, hydrogen is important product
Thing, meanwhile, hydrogen is again important industrial chemicals, be widely used in synthesis ammonia, be hydrocracked, in unifining process, petrochemical industry
Industry is always consumption hydrogen rich and influential family, and for many years, in petrochemical industry, supply falls short of demand always for hydrogen, with the exacerbation of feedstock oil and right
The raising of OR Octane Requirements, the disparities between supply and demand of hydrogen can be protruded more.
If with natural gas (or oil) come hydrogen manufacturing, not only complex process, and also need to consume substantial amounts of resource and energy；Separately
Outward, oil secondary operation (such as catalytic reforming, be hydrocracked, hydrofinishing and catalytic cracking) during, due to occurring one
The chemical reactions such as serial complicated cracking, isomerization, aromatisation, hydrogen migration and dehydrogenation, so, can give off again substantial amounts of hydrogeneous
Gas, if without suitable recovery method, flare system have to be sent to and burnt, in order to make rational use of resources, energy saving and
Environmental protection, best bet is recycled from suitable recovery method.
Hydrogen membrane separation technique is increasingly received significant attention as the extraordinary recovery method of one of which.Organic film
Separation Technique of Hydrogen Gas is more ripe, but is not suitable for complex environment (organic hydrocarbon, soda acid, temperature are high), when being applied to hydrogen recovery,
Complex pretreatment need to be carried out to unstripped gas, waste substantial amounts of energy, and flow is complicated, does not possess regeneration after pollution
Ability.And used as inoranic membrane used in hydrogen recycle, it is typically represented as Carbon Molecular Sieve Membrane, because high suitable for high temperature
Pressure and complex environment, hydrogen recovery rate and purity are higher, and film regenerability is good, is increasingly favored by researcher；Mesh
The main difficult technical of preceding influence Carbon Molecular Sieve Membrane industrial applications is that the membrane material of the membrane module consuming of equal volume is excessive, because
This can bring the decline of economic benefit.
The information for being disclosed in the background section is merely intended to deepen the understanding to general background technology of the invention, and
In being not construed as recognizing or imply in any form information structure prior art known to those skilled in the art.
The content of the invention
It is an object of the invention to provide membrane module, the hydrogen gas recovering device based on membrane module and Hydrogen Separation method,
Largely solve above mentioned problem.
It is an object of the invention to provide a kind of membrane module.
The second object of the present invention is to provide a kind of hydrogen gas recovering device based on membrane module.
The third object of the present invention is to provide a kind of Hydrogen Separation method.
On the one hand, the membrane module that the present invention is provided includes multiple Carbon Molecular Sieve Membranes, and each described Carbon Molecular Sieve Membrane is into pipe
Shape, and the Carbon Molecular Sieve Membrane of many tubuloses ties up to form membrane module；
The Carbon Molecular Sieve Membrane includes ceramic membrane and is plated in the film plating layer on its surface, the plating of each Carbon Molecular Sieve Membrane
Film layer is exposed at outer surface.
Further, the ceramic membrane vertical direction includes separating layer, transition zone and supporting layer successively；
The separating layer, transition zone and supporting layer are made by aluminum oxide.
Further, entered by sealing packed layer fitted seal glue between the Carbon Molecular Sieve Membrane of the tubulose of arbitrary neighborhood
Row is tied up.
Further, the sealing packed layer is using ceramics, glass, resin, rubber, carclazyte, carbon black, titanium dioxide or asbestos
Material.
Further, the fluid sealant is plasticizer, curing agent or accelerator.
Further, the quantity of the Carbon Molecular Sieve Membrane of the tubulose is 5-300 roots, and bore is 0.1-5mm, pipe external diameter
0.5-8mm, pipe range is 700-1000mm.
On the other hand, the present invention also provides a kind of hydrogen gas recovering device based on membrane module, including raw material gas tank, temperature control set
Standby and described membrane module, the raw material gas tank, temperature control device sequentially pass through the first pipeline and are connected with the membrane module, and institute
Membrane module is stated to be connected with tail gas recycle tank and hydrogen recycling can respectively.
Further, the outside of the membrane module is arranged with housing, and the housing side is respectively equipped with and raw material gas tank
The unstripped gas entrance being connected and the offgas outlet being connected with tail gas recycle tank, the top or bottom of the housing are provided with and hydrogen
The hydrogen outlet that gas recycling can is connected.
Further, the raw material gas tank is also connected with tail gas recycle tank by the second pipeline, and first pipeline
Regulating valve is equipped with the second pipeline.
Finally, the present invention also provides a kind of Hydrogen Separation method, using the described hydrogen gas recovering device based on membrane module,
Mainly include the following steps that：
Step one：The regulating valve on the first pipeline is opened, the regulating valve closed on the second pipeline, by unstripped gas via raw material
Delivered in cylinders is to the first pipeline；
Step 2：Adjustment temperature control device, by unstripped gas temperature stabilization after, be delivered to membrane module；
Step 3：After membrane module carries out Hydrogen Separation, the hydrogen of purification is reclaimed unstripped gas via hydrogen recycling can, tail
Gas is reclaimed via tail gas recycle tank.
Beneficial effects of the present invention：
On the one hand, the present invention provide membrane module, it includes multiple Carbon Molecular Sieve Membranes, each described Carbon Molecular Sieve Membrane into
Tubulose, and the Carbon Molecular Sieve Membrane of many tubuloses ties up to form membrane module；The Carbon Molecular Sieve Membrane includes ceramic membrane and plating
In the film plating layer on its surface, the film plating layer of each Carbon Molecular Sieve Membrane is exposed at outer surface；Wherein Carbon Molecular Sieve Membrane is tubulose, and
And using the outer plated film of pipe, it is possible to greatly improve, the every effective surface area of the Carbon Molecular Sieve Membrane of tubulose, the film group of equal size
Part is accomplished by the Carbon Molecular Sieve Membrane of less tubulose, saves materials；And manage outer plated film so that pipe inner volume is larger, also may be used
To provide loading density high.
On the other hand, the hydrogen gas recovering device based on membrane module that the present invention is provided, it includes described membrane module, therefore
It has all advantages of Carbon Molecular Sieve Membrane, does not just repeat herein.
Finally, the present invention also provides a kind of Hydrogen Separation method, using the described hydrogen gas recovering device based on membrane module,
Therefore it has all advantages of the hydrogen gas recovering device based on membrane module, does not just repeat herein.
Brief description of the drawings
In order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art, below will be to specific
The accompanying drawing to be used needed for implementation method or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the explosive view of the Carbon Molecular Sieve Membrane that the embodiment of the present invention one is provided；
Fig. 2 is the top view of the Carbon Molecular Sieve Membrane of the tubulose that the embodiment of the present invention one based on Fig. 1 is provided；
Fig. 3 is the structural representation of the membrane module that the embodiment of the present invention one based on Fig. 1 and Fig. 2 is provided；
Fig. 4 is the structural representation outside the membrane module that the embodiment of the present invention two based on Fig. 1-Fig. 3 is provided；
Fig. 5 is the structural representation of the hydrogen gas recovering device based on membrane module that the embodiment of the present invention two based on Fig. 4 is provided
Figure.
Icon：10- film plating layers；11- separating layers；12- transition zones；13- supporting layers；14- Carbon Molecular Sieve Membranes；15-
Sealing packed layer；16- unstripped gas entrances；17- offgas outlets；18- hydrogen outlets；19- raw material gas tanks；20- temperature controls set
It is standby；The pipelines of 21- first；The pipelines of 22- second；23- hydrogen recycling cans；24- tail gas recycle tanks；25- regulating valves；26- films
Component.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with accompanying drawing, it is clear that described implementation
Example is a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
In the description of the invention, it is necessary to explanation, term " " center ", " on ", D score, "left", "right", " vertical ",
The orientation or position relationship of the instruction such as " level ", " interior ", " outward " be based on orientation shown in the drawings or position relationship, merely to
Be easy to the description present invention and simplify describe, rather than indicate imply signified device or element must have specific orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.Additionally, term " first ", " second ",
" the 3rd " is only used for describing purpose, and it is not intended that indicating or implying relative importance.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Company ", " connection " should be interpreted broadly, for example, it may be being fixedly connected, or being detachably connected, or be integrally connected；Can
Being to mechanically connect, or electrically connect；Can be joined directly together, it is also possible to be indirectly connected to by intermediary, Ke Yishi
Two connections of element internal.For the ordinary skill in the art, with concrete condition above-mentioned term can be understood at this
Concrete meaning in invention.
Fig. 1 is the explosive view of the Carbon Molecular Sieve Membrane that the embodiment of the present invention one is provided；Fig. 2 is the present invention implementation based on Fig. 1
The top view of the Carbon Molecular Sieve Membrane of the tubulose that example one is provided；Fig. 3 is the film that the embodiment of the present invention one based on Fig. 1 and Fig. 2 is provided
The structural representation of component；Fig. 4 is the structural representation outside the membrane module that the embodiment of the present invention two based on Fig. 1-Fig. 3 is provided
Figure；Fig. 5 is the structural representation of the hydrogen gas recovering device based on membrane module that the embodiment of the present invention two based on Fig. 4 is provided.
Embodiment one
As Figure 1-3, it is many that the Carbon Molecular Sieve Membrane 14 that the present embodiment is provided includes that the membrane module 26 that the present invention is provided includes
Individual Carbon Molecular Sieve Membrane 14, each described Carbon Molecular Sieve Membrane 14 is tied up into tubulose, and many Carbon Molecular Sieve Membranes of the tubulose 14
Form membrane module 26；The Carbon Molecular Sieve Membrane 14 includes ceramic membrane and is plated in the film plating layer 10 on its surface, and each described carbon divides
The film plating layer 10 of sub- sieve membrane 14 is exposed at outer surface.
It is pointed out that film plating layer 10 is polymeric membrane, it is preferable that polymeric membrane is porous polymeric films.Porous is gathered
It is a kind of high molecular film material to close film, and the micropore of many penetrability is distributed with polymer thin film, is divided into plurality of specifications.Often
It is employed in the devices such as infiltration, filtration.The micropore gross area accounts for the 80% of the film gross area, and hole is through uniform in size.Porous polymerizing
The species of film has cellulose acetate film, nitrocellulose membrane, acetate fiber, cellulose nitrate mixed ester film, PA membrane, polytetrafluoroethyl-ne
Alkene film, polycarbonate membrane, PS membrane etc..The manufacture craft (such as cellulose mixed esters film) of polymeric membrane：Raw material is dissolved in solvent, and
Pore-foaming agent and some additives are added, at certain temperature and damp condition, is prepared with casting method.
It is pointed out that Carbon Molecular Sieve Membrane 14 is with high molecular polymer as presoma, to be commercialized porous ceramic film
It is carrier, by the high-performance separation membrane layer formed after the processes such as film, pretreatment, pyrolysis charring, post processing, ceramic monolith makes
The mechanical strength for obtaining whole Carbon Molecular Sieve Membrane is greatly improved.Film layer is coated with, in ceramic membrane carrier outer surface, to effectively reduce
The volume of membrane module, saves materials.
It may also be noted that Carbon Molecular Sieve Membrane 14 is pyrolyzed filming technology using high molecular polymer, using vacuum/inertia
The method of pyrolysis, plated film is carried out on the surface of ceramic membrane so that the mechanical strength of whole Carbon Molecular Sieve Membrane 14 is greatly improved.Carbon point
Sub- sieve membrane 14 belongs to one kind of inoranic membrane, and inoranic membrane refers to the ceramic membrane with sieve effect, Carbon Molecular Sieve Membrane 14, metal film
(porous symmetric membrane and asymmetric membrane obtained in alumilite process) and micropore glass.Aperture at 5-10 μm, can filtered water, solvent,
Solute, ion and small molecule, can retain colloid, bacterium, suspension, biological products and macromolecular, and can obtain reaction and separate
The multiple performance being combined.It is resistant to the high temperature of 1000K, antimicrobial erosion and chemical attack.Can be cleaned multiple times, but mouldability
Difference, is hit frangible, and porosity is low.Microfiltration membranes typically can be obtained, preparation method has solid particles sintering process, and also referred to as suspend grain
Sub- method；Metal alumilite process and sol-gal process.It is mainly used in micro-filtration, its particular product can be used for ultrafiltration.
It may also be noted that the membrane module 26 that the present embodiment is provided, it includes multiple Carbon Molecular Sieve Membranes 14, described in each
Carbon Molecular Sieve Membrane 14 ties up to form membrane module 26 into tubulose, and many Carbon Molecular Sieve Membranes of the tubulose 14；The carbon molecule
Sieve membrane 14 includes ceramic membrane and is plated in the film plating layer 10 on its surface, and the film plating layer 10 of each Carbon Molecular Sieve Membrane 14 exposes outside
Surface；Wherein Carbon Molecular Sieve Membrane 14 is tubulose, and using the outer plated film of pipe, it is possible to greatly improve, the every carbon molecule of tubulose
The effective surface area of sieve membrane 14, the membrane module 26 of equal size is accomplished by the Carbon Molecular Sieve Membrane 14 of less tubulose, saves use
Material；And manage outer plated film so that pipe inner volume is larger, it is also possible to provide loading density high.
Specifically, each concrete structure below for Carbon Molecular Sieve Membrane in the present embodiment 14 elaborates：
In the present embodiment, the ceramic membrane vertical direction includes separating layer 11, transition zone 12 and supporting layer 13 successively；
The separating layer 11, transition zone 12 and supporting layer 13 are made by aluminum oxide.
It is pointed out that ceramic membrane surface carries out plated film, then Carbon Molecular Sieve Membrane 14 is constituted.Carbon Molecular Sieve Membrane 14 has height
Mechanical strength, be applicable to HTHP and air velocity occasion higher.The thickness of supporting layer 13 is 0.5-2mm, permeability hole
Aperture is 0.1-1 μm；20-60 μm of 12 thickness of transition zone, permeability hole aperture is 50-100nm；The thickness 0.5-3 μ of separating layer 11
M, permeability hole aperture is 5-50nm；0.05-0.5 μm of 10 thickness of film plating layer, permeability hole aperture is 0.4-5nm.Permeability hole is wedge
Shape structure.
In the present embodiment, coordinate close by sealing packed layer 15 between the Carbon Molecular Sieve Membrane 14 of the tubulose of arbitrary neighborhood
Sealing is tied up.
In the present embodiment, it is described sealing packed layer 15 using ceramics, glass, resin, rubber, carclazyte, carbon black, titanium dioxide or
Asbestos material.
In the present embodiment, the fluid sealant is plasticizer, curing agent or accelerator.
It is pointed out that many Carbon Molecular Sieve Membranes of tubulose 14 are moulded by sealing the fitted seal glue of packed layer 15
Envelope, its bonding effect preferably, is easy to the Hydrogen Separation in later stage, prevents plastic packaging effect difference from causing gas leak.
In the present embodiment, the quantity of the Carbon Molecular Sieve Membrane 14 of the tubulose is 5-300 roots.
In the present embodiment, the bore of the Carbon Molecular Sieve Membrane 14 of the tubulose is 0.1-5mm, pipe external diameter 0.5-8mm, pipe
A length of 700-1000mm.
Embodiment two
As illustrated in figures 4-5, on the basis of embodiment one, the present embodiment also provides a kind of hydrogen based on membrane module and reclaims
Device, including raw material gas tank 19, temperature control device 20 and described membrane module 26, the raw material gas tank 19, temperature control device 20 and institute
State membrane module 26 and sequentially pass through the first pipeline 21 and be connected, and the membrane module 26 is reclaimed with tail gas recycle tank 24 and hydrogen respectively
Tank 23 is connected.
It is pointed out that the hydrogen gas recovering device based on membrane module that the present embodiment is provided, it includes described carbon point
Sub- sieve membrane 14, therefore it has all advantages of Carbon Molecular Sieve Membrane 14, does not just repeat herein.
Specifically, each concrete structure below for the hydrogen gas recovering device based on membrane module in the present embodiment makees detailed
Explanation：
In the present embodiment, the outside of the membrane module 26 is arranged with housing, and the housing side is respectively equipped with and raw material
Unstripped gas entrance 16 that gas tank 19 is connected and the offgas outlet 17 being connected with tail gas recycle tank 24, the top of the housing or
Bottom is provided with the hydrogen outlet 18 being connected with hydrogen recycling can 23.
It is pointed out that according to the specification of the good membrane module 26 of plastic packaging, the making of housing is carried out, and fitted seal is filled
After layer 15, membrane module 26 is mounted to；Sealing packed layer 15 is special exotic material, can be rubber, asbestos or graphite etc..
In the present embodiment, the raw material gas tank 19 is also connected with tail gas recycle tank 24 by the second pipeline 22, and described
Regulating valve 25 is equipped with first pipeline 21 and the second pipeline 22.
It is pointed out that when needing to carry out Hydrogen Separation, the regulating valve 25 on the first pipeline 21 is opened, gradually
The regulating valve 25 closed on the second pipeline 22, carries out Hydrogen Separation；When need not temporarily carry out Hydrogen Separation, the first pipe
Regulating valve 25 on line 21 is closed, and opens the regulating valve 25 on the second pipeline 22, directly derives unstripped gas；Two pipelines and tune
The setting of valve 25 is saved, facilitates two kinds of different working conditions on same production line, improve operating efficiency.
The flow that this is based on the hydrogen gas recovering device of membrane module is as follows：
After unstripped gas is through the equilibrium temperature of temperature control device 20, into membrane module 26；Product gas are the hydrogen after purification, from film group
Part 26 is collected after discharging；Tail gas is to remove the gas after hydrogen, is collected from after the discharge of membrane module 26 and recycled；Membrane module 26
By-pass is set, is used during beneficial to shutting down.Unstripped gas temperature is -50-600 DEG C, and the both sides differential pressure of membrane module 26 is 0-
8.0MPa。
Embodiment three
On the basis of embodiment two, the present embodiment also provides a kind of Hydrogen Separation method, mainly includes the following steps that：
Step one：The regulating valve 25 on the first pipeline 21 is opened, the regulating valve 25 closed on the second pipeline 22, by unstripped gas
The first pipeline 21 is delivered to via raw material gas tank 19；
Step 2：Adjustment temperature control device 20, by unstripped gas temperature stabilization after, be delivered to membrane module 26；
Step 3：After membrane module 26 carries out Hydrogen Separation, the hydrogen of purification is via hydrogen recycling can 23 times for unstripped gas
Receive, tail gas is reclaimed via tail gas recycle tank 24.
The present embodiment also provides a kind of experimental procedure of Hydrogen Separation：
1st, raw material source of the gas is got out, regulating valve 25 and raw material pressure-reducing valve on the first pipeline 21 is opened, unstripped gas is introduced
System, boosts to system, when system pressure boosts to 0.7MPa, the regulating valve 25, tail gas on the first pipeline 21 of adjustment
Valve and product air valve, make the stability of flow of pressure stability to 0.7Mpa, unstripped gas observe 10min in 833cc/min, and system is steady
After fixed, difference record start time, room temperature, flow and pressure and other parameters；Unstripped gas, hydrogen and tail gas are connected to chromatogram successively
Instrument, on-line analysis is carried out to hydrogen purity at room temperature.
2nd, the temperature of setting temperature control device 20 controls heating rate≤5 DEG C/min to 150 DEG C, and unstripped gas is heated into 150
DEG C, the regulating valve 25 on big first pipeline 21 is opened in temperature-rise period in good time, it is ensured that system pressure is stably maintained at 0.7MPa；System
After stabilization 10min, unstripped gas, hydrogen and tail gas are connected to chromatogram by the parameter such as record time, pressure, flow and temperature successively
Instrument, on-line analysis is carried out to the hydrogen purity at 150 DEG C.
3rd, the temperature of setting temperature control device 20 controls heating rate≤5 DEG C/min to 250 DEG C, and unstripped gas is heated into 250
DEG C, the regulating valve 25 on big first pipeline 21 is opened in temperature-rise period in good time, it is ensured that system pressure is stably maintained at 0.7MPa；System
After stabilization 10min, unstripped gas, hydrogen and tail gas are connected to chromatogram by the parameter such as record time, pressure, flow and temperature successively
Instrument, on-line analysis is carried out to the hydrogen purity at 250 DEG C.
Via the experimental result that above-mentioned Hydrogen Separation step is obtained：
To sum up, beneficial effects of the present invention：
First, the present invention is using ceramic membrane as substrate, it can be ensured that Carbon Molecular Sieve Membrane 14 has mechanical strength high when in use；
2nd, the present invention uses vacuum inert high temperature pyrolysis coating process, it can be ensured that permeability hole pore size control is evenly distributed, gas
Body separating effect is more preferable；
3rd, the Carbon Molecular Sieve Membrane 14 of tubulose of the present invention is in composite construction, and the wedge shaped structure of permeability hole can increase flux, and
Carbon Molecular Sieve Membrane 14 is difficult to be blocked because of impurity；
4th, using outer surface plated film, maximizing increases efficiently separating for the Carbon Molecular Sieve Membrane 14 of single tubulose to the present invention
Surface area；
5th, the Carbon Molecular Sieve Membrane 14 of tubulose of the present invention ties up flip-clip, can be by the carbon molecule of greater number of tubulose
The integrated plastic packaging of sieve membrane 14, increases surface area, for industrialization lays the foundation；
6th, the coefficient of thermal expansion of the capsulation material of inventive film component 26 is consistent with base material, it is ensured that heat when it is used
Swollen and mechanical strength, selects with specific reference to use environment；
7th, the sealing packed layer 15 of membrane module of the invention 26 can tolerate high temperature, and high resilience, it is ensured that sealing
Energy；
8th, the implementing process simple flow that the present invention is provided, suitable environment is extensive.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
Pipe has been described in detail with reference to foregoing embodiments to the present invention, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. a kind of membrane module, it is characterised in that including multiple Carbon Molecular Sieve Membranes, each described Carbon Molecular Sieve Membrane into tubulose, and
The Carbon Molecular Sieve Membrane of many tubuloses ties up to form membrane module；
The Carbon Molecular Sieve Membrane includes ceramic membrane and is plated in the film plating layer on its surface, the film plating layer of each Carbon Molecular Sieve Membrane
It is exposed at outer surface.
2. membrane module according to claim 1, it is characterised in that the ceramic membrane vertical direction include successively separating layer,
Transition zone and supporting layer；
The separating layer, transition zone and supporting layer are made by aluminum oxide.
3. membrane module according to claim 1, it is characterised in that between the Carbon Molecular Sieve Membrane of the tubulose of arbitrary neighborhood
Tied up by sealing packed layer fitted seal glue.
4. membrane module according to claim 3, it is characterised in that the sealing packed layer using ceramics, glass, resin,
Rubber, carclazyte, carbon black, titanium dioxide or asbestos material.
5. membrane module according to claim 3, it is characterised in that the fluid sealant is plasticizer, curing agent or accelerator.
6. membrane module according to claim 1, it is characterised in that the quantity of the Carbon Molecular Sieve Membrane of the tubulose is 5-300
Root, bore is 0.1-5mm, pipe external diameter 0.5-8mm, and pipe range is 700-1000mm.
7. a kind of hydrogen gas recovering device based on membrane module, it is characterised in that including raw material gas tank, temperature control device and claim
Membrane module described in any one of 3-6, the raw material gas tank, temperature control device sequentially pass through the first pipeline and are connected with the membrane module
Lead to, and the membrane module is connected with tail gas recycle tank and hydrogen recycling can respectively.
8. the hydrogen gas recovering device based on membrane module according to claim 7, it is characterised in that the outside of the membrane module
Be arranged with housing, and the housing side be respectively equipped with the unstripped gas entrance that is connected with raw material gas tank and with tail gas recycle tank phase
The offgas outlet of connection, the top or bottom of the housing are provided with the hydrogen outlet being connected with hydrogen recycling can.
9. the hydrogen gas recovering device based on membrane module according to any one of claim 7 or 8, it is characterised in that the original
Material gas tank is also connected with tail gas recycle tank by the second pipeline, and is equipped with regulation on first pipeline and the second pipeline
Valve.
10. a kind of Hydrogen Separation method, it is characterised in that the hydrogen based on membrane module described in application claim 9 reclaims dress
Put, mainly include the following steps that：
Step one：The regulating valve on the first pipeline is opened, the regulating valve closed on the second pipeline, by unstripped gas via raw material gas tank
It is delivered to the first pipeline；
Step 2：Adjustment temperature control device, by unstripped gas temperature stabilization after, be delivered to membrane module；
Step 3：After membrane module carries out Hydrogen Separation, the hydrogen of purification is reclaimed unstripped gas via hydrogen recycling can, tail gas warp
Reclaimed by tail gas recycle tank.
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Effective date of registration: 20170807 Address after: 225300, building 2, building 818, 7 Longfeng Road, new energy industry zone, Hailing District, Jiangsu, Taizhou, 212 Applicant after: JIANGSU SAIRUI MAIKE NEW MATERIAL CO.,LTD. Address before: 310000 room 4, building 20, No. 242 Longtan Road, Hangzhou District, Yuhang, Zhejiang Applicant before: HANGZHOU RUIYUTONG MEMBRANE TECHNOLOGY Co.,Ltd. |
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Application publication date: 20170620 |