CN105457501A - Preparation method of efficient gas separation membrane - Google Patents
Preparation method of efficient gas separation membrane Download PDFInfo
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- CN105457501A CN105457501A CN201510961395.6A CN201510961395A CN105457501A CN 105457501 A CN105457501 A CN 105457501A CN 201510961395 A CN201510961395 A CN 201510961395A CN 105457501 A CN105457501 A CN 105457501A
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- 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
-
- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0083—Thermal after-treatment
-
- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
-
- 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
- B01D2323/00—Details relating to membrane preparation
- B01D2323/30—Cross-linking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/36—Introduction of specific chemical groups
Abstract
The invention belongs to the technical field of gas separation membranes, in particular to a preparation method of an efficient gas separation membrane based on transfer promotion and a molecular sieve selective permeability mechanism. According to the preparation method provided by the invention, through introducing a functional group and a molecular sieve onto a reverse osmosis base membrane, a certain dose of additive is introduced, and then post-treatment is performed at certain temperature. Through regulating a membrane structure from different levels, the synergistic effect of multiple choices is realized, so as to improve the performance of the separation membrane. The preparation method provided by the invention has the advantages that through the method of introducing the functional group and the molecular sieve, a reactive choice mechanism and a diffusion choice mechanism can be realized at the same time, and fine adjustment on the membrane structure can also be realized, a gas permeation passage is formed, the preparation of the efficient gas separation membrane can be realized under normal conditions without needing to change the preparation procedures of a common composite separation membrane; moreover, compared with the prior art, the gas separation membrane prepared by the preparation method has extremely high separation factors, relatively good reproducibility, and low preparation cost.
Description
Technical field
The invention belongs to gas separaion technical field of membrane, specifically refer to a kind of based on Faciliated diffusion and molecular sieve efficient gas diffusion barrier selecting mechanism and preparation method thereof.
Technical background
The gaseous jet simulation research of China starts from early 1980s, and it is most widely used or it is for CO
2separation.As oil field high pressure injects CO
2tertiary oil recovery technique, after crude oil goes out well head, containing 80%CO in associated gas
2, must separation and recovery be concentrated into more than 95% and refill in oil well again and recycle.And for example flue gas CO
2enrichment etc., therefore UF membrane becomes more general in the future, becomes the dense CO of economically feasible collection
2mode.And membrane separation process has the advantages such as the high and low energy consumption of separative efficiency, easy and simple to handle, environmental friendliness and floor space are little, increasing scholar is both at home and abroad made to drop into the research of this respect.
China's gas separation membrane product is single, and industry size is little, and application is not also in full swing.Particularly in recent years, the research of China to the modification this respect of the Material selec-tion of gas separation membrane and isolating construction is very active, but up to the present, these researchs are also just in laboratory stage, the report of not its large-scale production and application.And main research all concentrates on the heat treatment temperature etc. that uses new material, original material is introduced new group or change film forming in these, these be all single selection through the impact of mechanism on membrane separating property, seldom have scholar's research different choice through the impact of mechanism synergy on gas separaion membrane separating property.
Foreign country also has many scholars to be devoted to gas separation membrane to CO
2the research of separating property, but the report also not having its large-scale production and application.For the laboratory research stage, that does had reasonablely once made polymine/polyvinyl alcohol (PEI/PVA) blend film as Matsuyama etc., the amido contained in PEI can with CO
2reaction forms carbamate, to CO
2there is Faciliated diffusion effect.Mutually being wound around by polymer support and PVA chain makes carrier be fixed in film, blend film after 160 DEG C of heat treatment, CO
2/ N2 separation reaches as high as 230.And for example amido is incorporated into cross-linked type polyethylene alcohol (PVA) polymer film by Huang etc., and the PVA polymer film after crosslinked demonstrates higher CO
2the heat endurance (170 DEG C) that/N2 is selective and higher, measures CO at 110 DEG C
2/ N2 separation can reach 493.Although the research before comparing, the separation increase rate of the gas separation membrane prepared by them is higher, its relatively low gas permeability coefficient, and it is used widely, that is far from being enough.And along with CO
2cause global warming constantly to aggravate, no matter for environmental angle or economic angle, research separation is large, the high-performance CO that seepage velocity is fast
2gas separation membrane realizes CO
2to catch be really extremely urgent.
Summary of the invention
The present invention aims to provide a kind of based on Faciliated diffusion and molecular sieve efficient gas diffusion barrier selecting mechanism and preparation method thereof, namely by reverse osmosis membrane surface recombination molecular sieve with promote the material that gas component is transmitted, and can effective separation of C O
2and N2, make CO
2can more than 500 be reached with the separation factor of N2.
The present invention is achieved through the following technical solutions:
A kind of based on Faciliated diffusion and molecular sieve efficient gas diffusion barrier selecting mechanism and preparation method thereof, it is characterized in that: on counter-infiltration basement membrane, introduce functional group and molecular sieve, can realization response simultaneously mechanism and diffusion be selected to select mechanism, the fine setting to membrane structure can also be realized, form gas infiltration lane.In order to make high molecular functional group better to fix, introducing the additive of doses, then carrying out post processing at a certain temperature.By from different levels comprehensive regulation membrane structure, realize multiple choices through the synergy of mechanism in film, thus improve diffusion barrier performance.
As preferably, the macromolecule with functional group that above-mentioned preparation method introduces has cellulose acetate, polyimides, fluoropolymer, polyvinyl alcohol, one or more in polymine, and the high molecule mass volumetric concentration introduced is 0.1 ~ 1.0%.As better selection, the macromolecule with functional group of introducing is polyvinyl alcohol and polymine.
As preferably, above-mentioned preparation method's Middle molecule sieve can be one or more of 3A, 4A, 5A or zeolite molecular sieve, and as more preferably selecting, the molecular sieve used is zeolite molecular sieve, and average pore size is at 0.3-1.0nm.
As preferably, the additive that above-mentioned preparation method introduces has glutaraldehyde, one or more of citric acid or maleic acid, and the mass body volume concentrations of additive is 1 ~ 10%.As better selection, selected additive is glutaraldehyde, and the mass body volume concentrations of glutaraldehyde is 2 ~ 8%.
As preferably, the post-processing temperature of above-mentioned efficient gas diffusion barrier is 50 DEG C-100 DEG C.As better selection, the post-processing temperature of efficient gas diffusion barrier is 70 DEG C-90 DEG C.
In the present invention, reverse osmosis membrane can be low-pressure reverse osmosis membrane, bitter reverse osmosis membrane or seawater film, the kind of film there is no direct impact to result of the present invention, therefore can select business reverse osmosis membrane or self-control, this also for being of the present inventionly commonly suitable for, carry out commercial applications and provide possibility.
Wherein introduce the high molecular polymer with functional group, because it is of a great variety, so inventor carries out Experimental Comparison from a large amount of kinds, polymine wherein and polyvinyl alcohol have better effect relative to other kind, and when mass body volume concentrations is 0.1 ~ 1%, especially, 0.2 ~ 0.8% time, its performance is more superior.
Additive in efficient divided gas flow diffusion barrier preparation process is crosslinking agent, and comprise one or more in citric acid, maleic anhydride, glutaraldehyde, preferred glutaraldehyde, especially glutaraldehyde mass concentration is 2 ~ 8% time, and its performance is more superior.
The post-processing temperature of gas separation membrane can be controlled by baking oven, and especially 70 DEG C-90 DEG C time, performance is comparatively superior.
Beneficial effect: adopt method described in this patent, by introducing the method for functional group and molecular sieve, can realization response simultaneously mechanism and diffusion be selected to select mechanism, the fine setting to membrane structure can also be realized, form gas infiltration lane, do not need the preparation section changing conventional composite separating film, the preparation of efficient gas diffusion barrier can be realized under normal conditions, and relative to the gas separation membrane prepared by prior art this patent, there is high separation factor, reappearance is better, and preparation cost is cheap.
Detailed description of the invention
Below the specific embodiment of the present invention is illustrated:
Following embodiment is only provided as and illustrates and non-limiting the present invention.
Reverse osmosis membrane used in following examples is self-control ultra-low-pressure reverse osmosis film.The film date of manufacture is less than 30 days to the experiment date, and period is stored in 1.5% aqueous solution of sodium bisulfite.Before being prepared gas separation membrane, reverse osmosis membrane being shifted to an earlier date 60min and is soaked in pure water.
In following examples, evaluation is made to two of gas separation membrane performances: CO
2gas permeation rate and N2 gas permeation rate.Gas test pressure during performance evaluation is 0.3MPa.
In following examples, gas transmision rate is that unit is Lm2h/Mpa through the gas volume of unit are gas separation membrane the unit interval in above-mentioned test process.
Embodiment 1
The polyvinyl alcohol of 0.1% is joined the glutaraldehyde containing 1%, 0.5%0.3nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.1% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 2200Lm2h/Mpa, N2 be 4Lm2h/Mpa, be separated N2 and CO
2separation factor reach 550.
Embodiment 2
The polyvinyl alcohol of 0.2% is joined the glutaraldehyde containing 3%, 0.8%0.3nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.3% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 1800Lm2h/Mpa, N2 be 1Lm2h/Mpa, be separated N2 and CO
2separation factor reach 1800.
Embodiment 3
The polyvinyl alcohol of 0.3% is joined the glutaraldehyde containing 3%, 0.8%0.3nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.3% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 1200Lm2h/Mpa, N2 be 1Lm2h/Mpa, be separated N2 and CO
2separation factor reach 1200.
Embodiment 4
The polyvinyl alcohol of 0.4% is joined the glutaraldehyde containing 3%, 0.6%0.6nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.4% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 800Lm2h/Mpa, N2 be 1Lm2h/Mpa, be separated N2 and CO
2separation factor reach 800.
Embodiment 5
The polyvinyl alcohol of 0.5% is joined the glutaraldehyde containing 4%, 0.8%0.6nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.5% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 1700Lm2h/Mpa, N2 be 2Lm2h/Mpa, be separated N2 and CO
2separation factor reach 850.
Embodiment 6
The polyvinyl alcohol of 0.6% is joined the glutaraldehyde containing 3%, 0.6%0.5nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.6% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 1500Lm2h/Mpa, N2 be 2Lm2h/Mpa, be separated N2 and CO
2separation factor reach 750.
Embodiment 7
The polyvinyl alcohol of 0.7% is joined the glutaraldehyde containing 5%, 0.8%0.7nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.5% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 830Lm2h/Mpa, N2 be 1Lm2h/Mpa, be separated N2 and CO
2separation factor reach 830.
Embodiment 8
The polyvinyl alcohol of 0.8% is joined the glutaraldehyde containing 5%, 0.5%0.8nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.7% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 1800Lm2h/Mpa, N2 be 3Lm2h/Mpa, be separated N2 and CO
2separation factor reach 600.
Embodiment 9
The polyvinyl alcohol of 0.9% is joined the glutaraldehyde containing 8%, 0.5%0.3nm in zeolite molecular sieve mixed solution, after mixing, be coated on counter-infiltration basement membrane, outwell unnecessary solution after 20s, dry in the shade, to be coated on the film that dries in the shade containing 0.8% aq. polyethyleneimine, after 30s, outwell unnecessary solution, and process 20min in 70 DEG C of baking ovens.The gas separation membrane that legal system is standby thus in the gas separaion test process of 0.3MPa, CO
2gas permeation rate be the gas permeation rate of 750Lm2h/Mpa, N2 be 1Lm2h/Mpa, be separated N2 and CO
2separation factor reach 750.
Claims (6)
1. a preparation method for efficient gas diffusion barrier, is characterized in that: on counter-infiltration basement membrane, introduce functional group and molecular sieve; First introduce the additive of doses, then carry out post processing at a certain temperature;
The macromolecular material of described introducing functional group refers to cellulose acetate, polyimides, fluoropolymer, polyvinyl alcohol, or one or more in polymine, and the mass body volume concentrations of the macromolecular material introduced is 0.1 ~ 1.0%;
Described molecular sieve is one or more of 3A, 4A, 5A or zeolite molecular sieve;
The additive of described introducing has glutaraldehyde, citric acid, or one or more of maleic acid, and the mass body volume concentrations of additive is 1 ~ 10%.
2. the preparation method of a kind of efficient gas diffusion barrier according to claim 1, is characterized in that: the macromolecular material introducing functional group refers to polyvinyl alcohol or polymine.
3. the preparation method of a kind of efficient gas diffusion barrier according to claim 1, is characterized in that: described molecular sieve is zeolite molecular sieve, and average pore size is at 0.3-1.0nm.
4. the preparation method of a kind of efficient gas diffusion barrier according to claim 1, it is characterized in that: described additive is glutaraldehyde, and the mass body volume concentrations of glutaraldehyde is 2 ~ 8%.
5. the preparation method of a kind of efficient gas diffusion barrier according to claim 1, is characterized in that: the post-processing temperature of above-mentioned efficient gas diffusion barrier is 50 DEG C-100 DEG C.
6. the preparation method of a kind of efficient gas diffusion barrier according to claim 5, is characterized in that: the post-processing temperature of above-mentioned efficient gas diffusion barrier is 70 DEG C-90 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107513877A (en) * | 2017-07-12 | 2017-12-26 | 马鞍山科信网络科技有限公司 | A kind of preparation method of succinic anhydride modified fiber air filter paper |
| CN107930406A (en) * | 2016-10-13 | 2018-04-20 | 北京工商大学 | A kind of faciliated diffusion type gas separation membrane material composition and preparation method |
| CN110227360A (en) * | 2019-06-06 | 2019-09-13 | 太原理工大学 | A kind of preparation method and application of blend film that adulterating lignosulfonates |
| CN112870992A (en) * | 2021-01-13 | 2021-06-01 | 同济大学 | Zeolite membrane and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112870992A (en) * | 2021-01-13 | 2021-06-01 | 同济大学 | Zeolite membrane and preparation method thereof |
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