CN103933877A - Blend membrane comprising polyvinyl acetate and polyether-b-polyamide, preparation thereof and applications thereof - Google Patents
Blend membrane comprising polyvinyl acetate and polyether-b-polyamide, preparation thereof and applications thereof Download PDFInfo
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- CN103933877A CN103933877A CN201310023952.0A CN201310023952A CN103933877A CN 103933877 A CN103933877 A CN 103933877A CN 201310023952 A CN201310023952 A CN 201310023952A CN 103933877 A CN103933877 A CN 103933877A
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- polyvinyl acetate
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Abstract
The invention relates to a blend membrane comprising polyvinyl acetate and polyether-b-polyamide, preparation thereof and applications thereof. The polyvinyl acetate (PVAc) and polyether-b-polyamide (Pebax) are adopted as raw materials of the membrane, and a gas separation membrane is prepared by a solution blending method. The blend membrane has advantages of a glassy-state polymer membrane and a rubbery-state polymer membrane. Acid gases such as CO2, H2S and SO2 preferentially permeate the blend membrane. The blend membrane has high separation performances for CO2/N2, SO2/N2, H2S/CH4, CO2/CH4, and other systems.
Description
Technical field
The present invention relates to gas separation membrane technical field, be specifically related to the polyamide blended film of a kind of polyvinyl acetate and polyethers-b-and preparation and application.
Background technology
Along with the industrialized development in the whole world, CO
2discharge capacity increase year by year, the greenhouse effects that cause and and then the environmental problem brought be also on the rise, CO
2trapping and seal the extensive concern that (CCS) is subject to people from all walks of life up for safekeeping.CCS process comprises from source of the gas carries out CO
2trapping, CO
2transportation and CO
2seal up for safekeeping, wherein trap 2/3 left and right that energy consumption accounts for CCS loopful energy consumption saving wheel, be the bottleneck of restriction CCS development, so the efficient CO of Development of Novel
2trapping technique is the key of CCS development.
At present, for CO
2the conventional method of gas separation mainly contains Physical Absorption method, chemical absorption method, pressure swing adsorption method and condensation at low temperature etc.It is high that chemical absorbing is removed degree, is widely used, and can be used for CO
2the processing of the gaseous mixture that dividing potential drop is lower, but the equipment of chemical absorbing is huge, energy consumption is high, complex process, and etching apparatus pipeline, absorbent toxicity is large, and easily degraded and loss are large; Physisorphtion requires CO
2dividing potential drop is higher, and removal degree is but not high, and the adsorption capacity of pressure-variable adsorption is limited, and pretreatment requires high, and two kinds of methods are mainly used in synthetic-ammonia transformation gas and refinery gas; The gas membrane Seperation Technology that starts from latter half in 20th century has the features such as energy consumption is low, easy to use, operating flexibility is large, operational reliability is high, during processing, there will not be high temperature or other extreme case, is one of emphasis of researching and developing in the high and new technology field of countries in the world special concern.
The industrial CO the most often using
2diffusion barrier is polymer membrane, but due to the impact of its material self property, the gas permeability of gas in polymer film and selectively have the upper limit, and gas permeability is large, selectively little, and vice versa.Therefore, exploitation has compared with atmospheric infiltration coefficient simultaneously and compared with the membrane material of high selectivity, becomes the goal in research in this field.The close CO that polyvinyl acetate (PVAc) is considered to up to the present found
2property is the strongest only contains C, H, the polymer of O, the close CO in its structure
2functional group's acetate groups contributes to CO
2gas dissolving therein, has improved CO
2dissolving selective.From this angle, PVAc can be used as separation of C O
2membrane material, but its mechanical strength is low, can not be separately for film preparation field.Select a kind of suitable membrane material with it blend be to use it for one of method of the fairly simple economy of film separation field.The block copolymer that contains ether oxygen groups that polyethers-b-polyamide (Pebax) is a kind of commercialization, it not only has good film forming, also has good acid and alkali resistance and organic solvent, and has very high thermally-stabilised and mechanical stability.So the method for research PVAc and Pebax blend, for preparation high-performance CO
2diffusion barrier, improves CO
2separative efficiency, has very strong practical significance.
Summary of the invention
The object of the present invention is to provide the polyamide blended film of a kind of polyvinyl acetate and polyethers-b-, its preparation and application; This blend film is a kind of CO of making
2, H
2s and SO
2than other gas (O
2, N
2and CH
4deng) diffusion barrier that can preferentially permeate, and to CO
2/ N
2, SO
2/ N
2, H
2s/CH
4, CO
2/ CH
4etc. system, keep higher separating property.
The invention provides the polyamide blended film of a kind of polyvinyl acetate and polyethers-b-, the membrane material of this blend film is polyvinyl acetate (PVAc) and polyethers-b-polyamide (Pebax), wherein the mass fraction of polyvinyl acetate in blend film is that 0.01%～99%(is preferably 5%～50%), all the other are polyethers-b-polyamide.
The polyamide blended film of polyvinyl acetate provided by the invention and polyethers-b-, the structural formula of described polyvinyl acetate (PVAc) is:
Its molecular weight ranges 980～585,000.
The polyamide blended film of polyvinyl acetate provided by the invention and polyethers-b-, described polyethers-b-polyamide (Pebax) is block copolymer, its structural formula is:
Wherein, PA is acid amides segment, and PE is polyether segment; The molecular weight of copolymer is decided by the content of PA and PE in copolymer molecule, the molecular weight ranges 300～15000 of PA segment in copolymer molecule, the molecular weight ranges 200～6000 of PE segment in copolymer molecule.
The polyamide blended film of polyvinyl acetate provided by the invention and polyethers-b-, described PA segment is nylon-6 (PA6), nylon-11 (PA11) or PA-12 (PA12); PE segment is PEO (PEO), PPOX (PPO) or polybutylene oxide (PTMO).
The present invention also provides the preparation method of a kind of described polyvinyl acetate and the polyamide blended film of polyethers-b-, selecting the polyvinyl acetate (PVAc) that contains acetate groups and the polyethers-b-polyamide (Pebax) that contains ether oxygen groups is membrane material, method by solution blending is prepared casting solution, then casting film-forming or apply film forming on dull and stereotyped filter membrane on glass plate; Concrete preparation process is as follows:
A) preparation of casting solution: first polyethers-b-polyamide Pebax is dissolved in dimethylacetylamide to the Pebax solution of preparation quality concentration 0.1～20%; To the polyvinyl acetate PVAc that adds required quality in solution, prepare homogeneous phase casting solution again, solution temperature is 70～110 ℃;
B) adopt the method for one or two or more kinds combination in standing, negative pressure or ultrasonic deaeration to carry out casting solution deaeration.
C) by the method for casting film-forming masking or prepare composite membrane by painting method coating on dull and stereotyped filter membrane on glass plate or tetrafluoro plate;
D) remove residual solvent in film.
The preparation method of described polyvinyl acetate provided by the invention and the polyamide blended film of polyethers-b-, the described step a) mass fraction of middle Pebax solution is preferably 0.1～8%.
The present invention also provides the application of described blend film, and this blend film can be used as gas separation membrane, can realize the separation process of the admixture of gas of gas with various component, mainly comprises CO
2and N
2, CO
2and CH
4, H
2s and CH
4, SO
2and N
2separation.
The application of described blend film provided by the invention, this blend film is applied to comprise the separated of admixture of gas that preferential infiltration gas and non-preferential infiltration gas form, thereby the separation that realizes preferential infiltration gas with remove; Preferential infiltration gas comprises CO
2, H
2s or SO
2in one or two or more kinds gas; Non-preferential infiltration gas comprises N
2, O
2, C1～C4 hydrocarbon gas in one or two or more kinds gas.
The application of described blend film provided by the invention, there is transition temperature in the performance of blend film, and the scope of transition temperature is 30～60 ° of C.
Concrete advantage of the present invention is as follows:
1, the polyvinyl acetate PVAc selecting and two kinds of organic matters of polyethers-b-polyamide Pebax contain respectively these two kinds of acetate groups and ehter bonds can improve CO
2dissolve optionally close CO
2functional group.
2, the blend film that prepared by the present invention is a kind of sour gas CO
2, H
2s and SO
2deng with respect to inert gas (O
2, N
2and CH
4deng) polymer blend membrane that can preferentially see through.
3, the blend film that prepared by the present invention has the advantage of glassy polymers film and rubbery feel polymer film concurrently.
4, by the method for blend, prepare PVAc/Pebax blend film, solved the low problem of PVAc mechanical strength.
5, in the present invention, the dissolving of polymer and blend are all physical processes, and operating condition is gentle, is easy to repetition, is conducive to industrialization.
Accompanying drawing explanation
Fig. 1 is the testing arrangement figure of the separated blend film of gas, in figure: (1) first valve; (2) second valves; (3) the 3rd valves; (4) the 4th valves; (5) the 5th valves; (6) the 6th valves; (7) the 7th valves; (8) the 8th valves; (9) the 9th valves; (10) 1L gas tank; (11) 50ml gas tank; (12) 100ml gas tank; (13) Pressure gauge; (14) pressure sensor; (15) osmotic cell;
Fig. 2 is several gas permeability coefficients and the temperature relation figure (5atm) of the prepared PVAc/Pebax1074 of embodiment 1 (1/1);
Fig. 3 is several gas permeability coefficients and the temperature relation figure (5atm) of the prepared PVAc/Pebax1074 of embodiment 2 (3/7);
Fig. 4 is several gas permeability coefficients and the temperature relation figure (5atm) of the prepared PVAc/Pebax1074 of embodiment 3 (1/9).
The specific embodiment
PVAc/Pebax blend film preparation process of the present invention is as follows:
A) preparation of casting solution: first polyethers-b-polyamide Pebax is dissolved in dimethylacetamide solvent to the Pebax solution of preparation quality concentration 0.1～20%; To the polyvinyl acetate PVAc that adds required quality in solution, prepare homogeneous phase casting solution again, solution temperature is 70～110 ℃;
B) casting solution deaeration (standing, negative pressure or ultrasonic deaeration);
C) by the method for casting film-forming masking or prepare composite membrane by painting method coating on dull and stereotyped filter membrane on glass plate;
D) residual solvent in vacuum removal film.
In the present invention, PVAc/Pebax blend film is separated for gas, and its permeance property obtains by equal-volume-transformation method, and flow chart as shown in Figure 1.During test, step is as follows:
A) (osmotic cell is that two chambers that are separated into by film form film to be packed into osmotic cell, each chamber is equipped with the pipe joint being connected with the external world) in after, close the 6th valve and the 9th valve, all the other valves are all opened, whole system is vacuumized, make it under vacuum state, maintain 12h.
B) by the first valve and the second valve, select suitable per-meate side volume, all the other valve Close Alls, open the 9th valve, and in 1L gas tank, blanketing gas regulates pressure, and regulates temperature by temperature control system.
C) in test process, open the 7th valve and the 8th valve, the pressure that records per-meate side by pressure sensor changes, and then calculates infiltration coefficient and the separation of gas in film.
In formula:
The infiltration coefficient Barrer[1Barrer=10 of P---gas in film
-10cm
3(STP) cm/ (cm
2scmHg)]
The volume cm of V---gas permeation side
3
A---effective film area, cm
2
Δ p---the pressure differential of film both sides, cmHg
The thickness of l-mono-film, cm
The temperature of T---osmotic cell, ℃
Dm---osmotic lateral pressure improves needed time of 1mmHg, s
P
a---the infiltration coefficient Barrer[1Barrer=10 of gas A in film
-10cm
3(STP) cm/ (cm
2scmHg)]
P
b---the infiltration coefficient Barrer[1Barrer=10 of gas B in film
-10cm
3(STP) cm/ (cm
2scmHg)]
α
a/B---separation
Below in conjunction with specific embodiment, the present invention is further detailed explanation, but the invention is not restricted to specific embodiment.
Embodiment 1:
By the Pebax1074(m (PEO) after 2.5 grams of vacuum drying: m (PA12)=55:45, mass ratio) be added in 95 grams of dimethylacetamide solvents, at 80 ℃ of temperature, stir 6h, form after the Polymer Solution of transparent and homogeneous, to the PVAc that adds 2.5 grams in Polymer Solution, continue to stir 2h, form again after the solution of transparent and homogeneous, carry out standing and defoaming, casting solution after deaeration is poured in the smooth iron hoop on clean horizontal glass plate, make casting solution uniform spreading on glass plate, glass sheet temperatures remains on 50 ℃, carry out solvent evaporates, the final film of coming into being that forms.The film of coming into being carefully takes off from glass plate, puts into vacuum drying oven, and dry 72h, removes residual solvent, PVAc/Pebax1074 (1/1) the blend homogeneous membrane that the mass ratio that obtains PVAc and Pebax1074 is 1:1, and test its permeance property.
The experimental result of table 1 embodiment 1 (25 ℃, 5atm)
Embodiment 2:
Pebax1074 after 3.5 grams of vacuum drying is added in 95 grams of dimethylacetamide solvents, at 80 ℃ of temperature, stir 6h, form after the Polymer Solution of transparent and homogeneous, to the PVAc that adds 1.5 grams in Polymer Solution, continue to stir 2h, form again after the solution of transparent and homogeneous, carry out ultrasonic deaeration, casting solution after deaeration is poured in the smooth iron hoop on clean horizontal glass plate, make casting solution uniform spreading on glass plate, glass sheet temperatures remains on 50 ℃, carries out solvent evaporates, the final film of coming into being that forms.The film of coming into being carefully takes off from glass plate, puts into vacuum drying oven, and dry 72h, removes residual solvent, PVAc/Pebax1074 (3/7) the blend homogeneous membrane that the mass ratio that obtains PVAc and Pebax1074 is 3:7, and test its permeance property.
The experimental result of table 2 embodiment 2 (25 ℃, 5atm)
Embodiment 3:
Pebax1074 after 4.5 grams of vacuum drying is added in 95 grams of dimethylacetamide solvents, at 85 ℃ of temperature, stir 6h, form after the Polymer Solution of transparent and homogeneous, to the PVAc that adds 0.5 gram in Polymer Solution, continue to stir 2h, form again after the solution of transparent and homogeneous, carry out negative pressure deaeration; Casting solution after deaeration is poured on tetrafluoro plate, made casting solution uniform spreading on tetrafluoro plate, glass sheet temperatures remains on 50 ℃, carries out solvent evaporates, the final film of coming into being that forms.The film of coming into being carefully takes off from glass plate, puts into vacuum drying oven, and dry 72h, removes residual solvent, the blend homogeneous membrane of the PVAc/Pebax1074 (1/9) that the mass ratio that obtains PVAc and Pebax1074 is 1:9, and test its permeance property.
The experimental result of table 3 embodiment 3 (25 ℃, 5atm)
Comparative example 1:
Table 4 is comparisons of the gas separating property of Pebax1074/PVAc blend film in the embodiment of the present invention 1,2,3 and pure Pebax1074 and pure PVAc film.
The permeance property comparison of table 4Pebax1074/PVAc blend film and Pebax1074 and PVAc homogeneous membrane (25 ℃, 5atm)
Between embodiment 1,2,3, make comparisons and can find out that the content of Pebax1074 has a certain impact to the performance of blend film, along with the content increase of Pebax1074, gas permeability coefficient obviously rises, and transition temperature reduces.
The infiltration coefficient of PVAc/Pebax1074 blend film is greater than the infiltration coefficient of pure PVAc film as can be seen from the comparative examples, is selectively greater than the selective of pure Pebax1074 film simultaneously, shows that this blend film has the advantage of glassy polymers film and rubbery feel polymer film concurrently.
Claims (11)
1. a polyvinyl acetate and the polyamide blended film of polyethers-b-, it is characterized in that: the membrane material of this blend film is polyvinyl acetate PVAc and polyethers-b-polyamide Pebax, wherein the mass fraction of polyvinyl acetate in blend film is 0.01%～99%, and all the other are polyethers-b-polyamide.
2. according to polyvinyl acetate described in claim 1 and the polyamide blended film of polyethers-b-, it is characterized in that: the structural formula of described polyvinyl acetate PVAc is:
Its molecular weight ranges 980～585,000.
3. according to polyvinyl acetate described in claim 1 and the polyamide blended film of polyethers-b-, it is characterized in that: described polyethers-b-polyamide Pebax is block copolymer, and its structural formula is:
Wherein, PA is acid amides segment, and PE is polyether segment; The molecular weight of copolymer is decided by the content of PA and PE in copolymer molecule, the molecular weight ranges 300～15000 of PA segment in copolymer molecule, the molecular weight ranges 200～6000 of PE segment in copolymer molecule.
4. according to polyvinyl acetate described in claim 3 and the polyamide blended film of polyethers-b-, it is characterized in that: described PA segment is nylon-6 (PA6), nylon-11 (PA11) or PA-12 (PA12); PE segment is PEO (PEO), PPOX (PPO) or polybutylene oxide (PTMO).
5. according to polyvinyl acetate described in claim 1 and the polyamide blended film of polyethers-b-, it is characterized in that: the mass fraction of described polyvinyl acetate in blend film is 5%～50%.
6. a preparation method for polyvinyl acetate and the polyamide blended film of polyethers-b-described in claim 1, is characterized in that: the method step is as follows:
A) preparation of casting solution: first polyethers-b-polyamide Pebax is dissolved in solvent to the Pebax solution of preparation quality concentration 0.1～20%; To the polyvinyl acetate PVAc that adds required quality in solution, prepare homogeneous phase casting solution again, solution temperature is 70～110 ℃;
B) casting solution deaeration;
C) by the method for casting film-forming masking or prepare composite membrane by painting method coating on dull and stereotyped filter membrane on glass plate or tetrafluoro plate;
D) remove residual solvent in film.
7. according to the preparation method of polyvinyl acetate described in claim 6 and the polyamide blended film of polyethers-b-, it is characterized in that: the solvent of the dissolving polyethers-b-polyamide of described step in a) is dimethylacetylamide.
8. according to the preparation method of polyvinyl acetate described in claim 6 and the polyamide blended film of polyethers-b-, it is characterized in that: the described step a) mass fraction of middle Pebax solution is 0.1～8%.
9. according to the preparation method of polyvinyl acetate described in claim 6 and the polyamide blended film of polyethers-b-, it is characterized in that: casting solution deaeration described step b) adopts one or two or more kinds combination in standing, negative pressure or ultrasonic deaeration.
10. the application of blend film described in claim 1～5 any one, is characterized in that: this blend film can be used as gas separation membrane, can realize the separation process of the admixture of gas of gas with various component.
11. according to the application of blend film described in claim 10, it is characterized in that: this blend film is applied to comprise the separated of admixture of gas that preferential infiltration gas and non-preferential infiltration gas form, thus the separation that realizes preferential infiltration gas with remove;
Preferential infiltration gas comprises CO
2, H
2s or SO
2in one or two or more kinds gas;
Non-preferential infiltration gas comprises N
2, O
2, C1～C4 hydrocarbon gas in one or two or more kinds gas.
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|---|---|---|---|
| CN201310023952.0A CN103933877A (en) | 2013-01-22 | 2013-01-22 | Blend membrane comprising polyvinyl acetate and polyether-b-polyamide, preparation thereof and applications thereof |
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|---|---|---|---|
| CN201310023952.0A CN103933877A (en) | 2013-01-22 | 2013-01-22 | Blend membrane comprising polyvinyl acetate and polyether-b-polyamide, preparation thereof and applications thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106582307A (en) * | 2017-02-17 | 2017-04-26 | 中国科学院大连化学物理研究所 | Blend membrane preparation method and application of blend membrane |
| CN110354702A (en) * | 2019-06-20 | 2019-10-22 | 郑州大学 | One kind being used for CO2/N2The mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof of gas separation |
| CN111542384A (en) * | 2017-05-30 | 2020-08-14 | 沙特阿拉伯石油公司 | Polymer blend membranes for acid gas separation |
| CN112023730A (en) * | 2020-09-18 | 2020-12-04 | 天津工业大学 | Preparation of block polyether amide-photosensitive copper organic framework film and gas separation application |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106582307A (en) * | 2017-02-17 | 2017-04-26 | 中国科学院大连化学物理研究所 | Blend membrane preparation method and application of blend membrane |
| CN106582307B (en) * | 2017-02-17 | 2019-05-07 | 中国科学院大连化学物理研究所 | A kind of application of the preparation method and blend film of blend film |
| CN111542384A (en) * | 2017-05-30 | 2020-08-14 | 沙特阿拉伯石油公司 | Polymer blend membranes for acid gas separation |
| CN111542384B (en) * | 2017-05-30 | 2022-06-07 | 沙特阿拉伯石油公司 | Polymer blend membranes for acid gas separation |
| CN110354702A (en) * | 2019-06-20 | 2019-10-22 | 郑州大学 | One kind being used for CO2/N2The mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof of gas separation |
| CN110354702B (en) * | 2019-06-20 | 2021-10-08 | 郑州大学 | For CO2/N2Mixed matrix membrane for gas separation and preparation method thereof |
| CN112023730A (en) * | 2020-09-18 | 2020-12-04 | 天津工业大学 | Preparation of block polyether amide-photosensitive copper organic framework film and gas separation application |
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Application publication date: 20140723 |