CN106422800B - A kind of multi-well high-throughput gas separation membrane and preparation method thereof - Google Patents
A kind of multi-well high-throughput gas separation membrane and preparation method thereof Download PDFInfo
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- CN106422800B CN106422800B CN201610866289.4A CN201610866289A CN106422800B CN 106422800 B CN106422800 B CN 106422800B CN 201610866289 A CN201610866289 A CN 201610866289A CN 106422800 B CN106422800 B CN 106422800B
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- 239000012528 membrane Substances 0.000 title claims abstract description 44
- 238000000926 separation method Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005266 casting Methods 0.000 claims abstract description 22
- 239000011521 glass Substances 0.000 claims abstract description 17
- 229920006393 polyether sulfone Polymers 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 239000004695 Polyether sulfone Substances 0.000 claims abstract description 9
- 230000004907 flux Effects 0.000 claims abstract description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 10
- 239000008103 glucose Substances 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 229940113088 dimethylacetamide Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 229920002492 poly(sulfone) Polymers 0.000 abstract description 10
- 239000000654 additive Substances 0.000 abstract description 9
- 230000000996 additive effect Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 9
- 150000004676 glycans Chemical class 0.000 abstract description 7
- 229920001282 polysaccharide Polymers 0.000 abstract description 7
- 239000005017 polysaccharide Substances 0.000 abstract description 7
- 150000002772 monosaccharides Chemical class 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 32
- 210000004379 membrane Anatomy 0.000 description 23
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 9
- 229930006000 Sucrose Natural products 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000005720 sucrose Substances 0.000 description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 2
- 210000002469 basement membrane Anatomy 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000008101 lactose Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000935 solvent evaporation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- WQZGKKKJIJFFOK-DVKNGEFBSA-N alpha-D-glucose Chemical group OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-DVKNGEFBSA-N 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 229910001872 inorganic gas Inorganic materials 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- -1 methyl siloxane Chemical class 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 125000000185 sucrose group Chemical group 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
-
- 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
- B01D53/228—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 characterised by specific membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- 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
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to UF membrane field more particularly to a kind of multi-well high-throughput gas separation membrane and preparation methods.A kind of multi-well high-throughput gas separation membrane preparation method, the film is using polysulfones or polyether sulfone as membrane material, using monosaccharide and/or polysaccharide as additive, it is made using phase inversion, preparation method includes the following steps: monosaccharide and/or the dissolution of polysaccharide additive in organic solvent, membrane material to be then added, stirs, it is allowed to be completely dissolved, casting solution is made；It takes appropriate casting solution to be put on glass plate, is struck off with scraper, glass plate is put into baking oven later, solvent is evaporated, obtain porous gas seperation film；The ratio between usage amount of additive and membrane material is 1:2 ~ 1:10 by mass percentage.Method of the invention to form cavernous structure inside film, reduces resistance to mass tranfer, improves gas flux.Meanwhile the compacted zone of film surface ensure that the highly selective of film.
Description
Technical field
The invention belongs to UF membrane field more particularly to a kind of multi-well high-throughput gas separation membrane and preparation methods.
Background technique
The flux magnitude and selectivity quality of seperation film determine whether the separating effect of membrane separation assemblies is excellent.High-throughput
Gas separation membrane can effectively reduce membrane area, reduce equipment investment expense, and gas-selectively it is excellent mean it is available
The higher product of purity.Polymeric membrane is because having many advantages, such as that manufacturing cost is low, structural controllability is strong, good film-forming property is widely used
In the preparation of gas separation membrane, but there is permeability and selective the phenomenon that mutually restricting in conventional polymeric membrane mostly, in order to protect
Higher gas-selectively is demonstrate,proved, the relatively low problem of the generally existing permeability of polymeric gas seperation film industrially used at present.
The separating property of film can be effectively improved by polymer modification or Development of Novel Organic inorganic film, however,
Gap between inorganic particle and membrane material will be greatly reduced the selectivity of composite membrane, serious to restrict the separation of organic and inorganic gas
The development of film.There are the problems such as at high cost, performance is unstable for polymer modification.Chinese patent CN102806024A discloses one kind
The preparation method of high osmosis dimethyl silicone polymer gas separation membrane, which first prepares crosslinking agent, then in catalyst
Under effect, hydroxyl-terminated injecting two methyl siloxane is mixed with crosslinking agent, chemically reacts, obtains casting solution.Then in high score
It forms a film on the porous basement membrane of son.Film properties made from this method are preferable, and mechanical stability is strong, but preparation process is complicated, at high cost.
Chinese patent CN102580580A discloses polyimide gas separating film and preparation method thereof, and this method utilizes γ
Ray radiation is modified polyimide film, is easier to realize industrialization.Development of Novel high throughput gas separation membrane, for gas
The development of separation membrane technology is of great significance.
The characteristics of gas separation membrane can be divided into dense form and porous type, dense film is that have highly selective, but component passes through
The infiltration rate of dense film is too low, and the preparation cost of film is higher, limits its industrial application.The performance and densification of perforated membrane
Film is different, and gas permeability is good compared with dense film, but selectivity is lower.
Summary of the invention
In order to solve the above technical problems, one object of the present invention provides a kind of multi-well high-throughput gas separation membrane preparation
Method reduces resistance to mass tranfer so that forming cavernous structure inside film, improves gas flux.Meanwhile the compacted zone of film surface guarantees
Film it is highly selective.Another object of the present invention is to provide the multi-well high-throughput gas point that above-mentioned method is prepared
From film.
In order to realize first above-mentioned purpose, present invention employs technical solutions below:
A kind of multi-well high-throughput gas separation membrane preparation method, the film using polysulfones or polyether sulfone as membrane material, with monosaccharide and/
Or polysaccharide is additive, is made using phase inversion, preparation method includes the following steps: to add monosaccharide and/or polysaccharide
Agent is dissolved in organic solvent, and membrane material is then added, and is stirred, is allowed to be completely dissolved, and casting solution is made；Appropriate casting solution is taken to put
Enter on glass plate, struck off with scraper, glass plate is put into baking oven later, solvent is evaporated, obtains porous gas point
From film；The ratio between usage amount of additive and membrane material is 1:2 ~ 1:10 by mass percentage.
Preferably, the usage amount of each component by mass percentage membrane material be 10-30%, organic solvent 70-85%,
Additive is 1-10%.As further preferably, membrane material is 16-28%, organic solvent to the usage amount of each component by mass percentage
For 75-80%, additive 1-10%.
Preferably, selected polyether sulfone model E6020P, polysulfones model A-300.
Preferably, selected monosaccharide is alpha-D-glucose or β-D-Glucose, selected polysaccharide is sucrose or lactose.
Preferably, evaporating temperature is 30-70 DEG C to casting solution in an oven.
Preferably, this method includes the following steps:
1) casting solution configures
Monosaccharide or polysaccharide are added in organic solvent, stirs, is allowed to sufficiently dissolve, polysulfones or polyethers is then added
Sulfone, heating, is sufficiently stirred and makes it completely dissolved, and forms polymer/solvent binary casting solution, and closed stand takes off under certain temperature
Bubble, can be prepared by required casting solution；
2) phase inversion prepares porous gas seperation film
After filtering by the complete casting solution of deaeration, it is scraped by scraping film device to the glass plate of clean dried, is put into baking oven
Middle progress solvent evaporation, makes solvent volatilize completely, and seperation film is made；Glass plate is soaked with water, carefully by film from glass plate
Removing is soaked for a period of time into the water with the solid-state glucose for film surface precipitation of going out.
Another object of the present invention is to provide the multi-well high-throughput gas separation membrane that above-mentioned method is prepared.
The present invention is using gas separation membrane prepared by above-mentioned technical solution, by one in glucose, sucrose and lactose
Kind is added in casting solution, so that generation is porous in film, resistance to mass tranfer is effectively reduced, improves gas flux.Gas separating experiment
Show compared to PES basement membrane, be added to after glucose, film is to H2And N2Flux 24.5% and 30% has been respectively increased, and select
Selecting property remains unchanged, and can should separate in industrial associated gas.
The beneficial effects of the present invention are: being dredged using the hydrophilies such as glucose, polysaccharide small organic molecule and polyether sulfone, polysulfones etc.
It is insoluble between aqueous organic polymer, porous gas seperation film is made by evaporation solvent method.In solvent evaporation process,
It generates and separates between added small organic molecule and polymer segment, control the dosage of micromolecule additive, can be prepared by
Surface compact and the internal porous gas seperation film containing hole, effectively improve the flux of gas molecule, while keeping high choosing
Selecting property.This method is simple and easy, can prepare the polyether sulfone or polysulfones gas of different flux and selectivity by changing reaction condition
Body seperation film, prepared gas separation membrane can be widely applied to the gas separation of industrial circle, such as CO in natural gas2Go
It removes, the separation of oxygen and nitrogen, the recycling of hydrogen etc. in air.
Detailed description of the invention
Fig. 1 is surface (left figure) and section (right figure) pattern of perforated membrane obtained in embodiment 1.
Fig. 2 is surface (left figure) and section (right figure) pattern of dense film obtained in embodiment 1.
Fig. 3 is surface (left figure) and section (right figure) pattern of perforated membrane obtained in embodiment 2.
Fig. 4 is surface (left figure) and section (right figure) pattern of perforated membrane obtained in embodiment 3.
Fig. 5 is surface (left figure) and section (right figure) pattern of perforated membrane obtained in embodiment 4.
Specific embodiment
Following example is not used to explain limiting the scope of the invention for illustrating the present invention.
Embodiment 1
2 g glucose are added in 80 g N-Methyl pyrrolidone organic solvents, is sufficiently stirred, is allowed to be completely dissolved,
Then 18 g polyether sulfones (E6020P) are added, are dissolved by heating in 60 DEG C.Object to be polymerized carries out constant temperature deaeration after being completely dissolved, it
Use scraper in the glass pane surface knifing of clean dried afterwards, then casting solution will be coated with the glass of casting solution with a thickness of 100 μm
Plate is put into baking oven in 40 DEG C of 24 h of evaporation, and taking-up obtains polyethersulfone porous membrane (its surface and cross-section morphology are shown in attached drawing 1).It should
Film is to N2Flux be 0.212 barrers, to H2Flux be 14.35 barrers, to CO2Flux be 132
barrers.It is to H2/N2And H2/CO2Selectivity be 67.7 and 9.19.Meanwhile the dense film without glucose also uses
Process above preparation, except that being free of glucose in formula.Its casting solution group becomes 18 g polyether sulfones (E6020P) and 82
G N-Methyl pyrrolidone.The surface of dense film and cross-section morphology are shown in attached drawing 2.Compared by Fig. 1 and Fig. 2 it is found that being added to grape
After sugar, the surface of film forms many concave surfaces, while occurring hole in film, and the concave surface of film surface is conducive to capture gas molecule,
What the hole in film reduced film reaches resistance, to improve the flux of film.Gas separating resulting shows dense film to H2、N2With
CO2Flux be respectively 77.2%, 82.3% and the 81.6% of perforated membrane.
Embodiment 2
4 g glucose are added to 78 g N, in N- dimethyl acetamide organic solvent, are sufficiently stirred, are allowed to completely molten
Solution, is then added 18 g polyether sulfones (E6020P), dissolves by heating in 60 DEG C.It is de- that object to be polymerized carries out constant temperature after being completely dissolved
Bubble, uses scraper in the glass pane surface knifing of clean dried later, then casting solution will be coated with casting solution with a thickness of 100 μm
Glass plate is put into baking oven in 50 DEG C of 24 h of evaporation, and taking-up obtains polyethersulfone porous membrane.The film is to N2Flux be 0.124
Barrers, to H2Flux be 11.23barrers, to CO2Flux be 92 barrers.It is to H2/N2And H2/CO2's
Selectivity is respectively 90.56 and 8.19.The surface of the film and cross-section morphology are shown in attached drawing 3.
Embodiment 3
8 g sucrose are added to 74 g N, in N- dimethyl acetamide organic solvent, is sufficiently stirred, is allowed to be completely dissolved,
Then 18 g polysulfones (A-300) are added, are dissolved by heating in 60 DEG C.Object to be polymerized carries out constant temperature deaeration after being completely dissolved, later
With scraper in the glass pane surface knifing of clean dried, then casting solution will be coated with the glass plate of casting solution with a thickness of 100 μm
It is put into baking oven in 70 DEG C of 24 h of evaporation, taking-up obtains polysulfone porous membrane.The surface of the film and cross-section morphology are shown in attached drawing 4.By
Figure can effectively increase the density and film section Hole quantity of film surface concave surface it is found that improving additive level, to improve
The separating effect of film.By gas separating resulting it is found that the film is to N2Flux be 0.186 barrers, to H2Flux be
17.11barrers to CO2Flux be 96.77 barrers.It is to H2/N2And H2/CO2Selectivity be respectively 91.98
With 5.66.
Embodiment 4
8 g sucrose are added in 74 g N-Methyl pyrrolidone organic solvents, is sufficiently stirred, is allowed to be completely dissolved, so
After 20 g polysulfones (A-300) are added, in 60 DEG C dissolve by heating.Object to be polymerized carries out constant temperature deaeration, Zhi Houyong after being completely dissolved
Scraper in the glass pane surface knifing of clean dried, then put the glass plate for being coated with casting solution with a thickness of 100 μm by casting solution
Enter in 70 DEG C of 24 h of evaporation in baking oven, taking-up obtains polysulfone porous membrane.By gas separating resulting it is found that the film is to N2Flux
For 0.116 barrers, to H2Flux be 12.52barrers, to CO2Flux be 91.65 barrers.It is to H2/N2
And H2/CO2Selectivity be respectively 107.9 and 7.32.The surface of the film and cross-section morphology are shown in attached drawing 5.
Claims (1)
1. a kind of multi-well high-throughput gas separation membrane preparation method, it is characterised in that: 4 g glucose are added to 78 g N, N-
It in dimethyl acetamide organic solvent, is sufficiently stirred, is allowed to be completely dissolved, 18 g E6020P polyether sulfones are then added, in 60 DEG C
It dissolves by heating, object to be polymerized carries out constant temperature deaeration after being completely dissolved, and the glass pane surface with scraper in clean dried is scraped later
Then the glass plate for being coated with casting solution is put into baking oven in 50 DEG C of 24 h of evaporation, taking-up is by film, casting solution with a thickness of 100 μm
Polyethersulfone porous membrane is made, the film is to N2Flux be 0.124 barrers, to H2Flux be 11.23barrers, to CO2
Flux be 92 barrers, to H2/N2And H2/CO2Selectivity be respectively 90.56 and 8.19.
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| CN201610866289.4A CN106422800B (en) | 2016-09-30 | 2016-09-30 | A kind of multi-well high-throughput gas separation membrane and preparation method thereof |
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| 添加剂对聚砜膜气体分离性能和结构的影响;孙爱玲等;《天津理工大学学报》;20140630;第30卷(第3期);第50-53页 |
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