CN105749769A - Preparation method and application of ionic liquid blended membrane - Google Patents
Preparation method and application of ionic liquid blended membrane Download PDFInfo
- Publication number
- CN105749769A CN105749769A CN201610235201.9A CN201610235201A CN105749769A CN 105749769 A CN105749769 A CN 105749769A CN 201610235201 A CN201610235201 A CN 201610235201A CN 105749769 A CN105749769 A CN 105749769A
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- ionic liquid
- polyoxyethylene
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- imidazole type
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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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/80—Block polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—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
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- 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
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- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
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- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method and application of an ionic liquid blended membrane and belongs to the technical field of gas separating membranes.The preparation method includes: preparing a polyoxyethylene-polycaprolactam segmented copolymer solution, and adding imidazole type room-temperature ionic liquid into the solution to obtain membrane casting liquid; drying at room temperature, and further drying under a vacuum condition to obtain the ionic liquid blended membrane.The preparation method and the application have the advantages that the preparation method is simple, and the ionic liquid is fixed in macromolecular chains, thereby being low in loss rate; the composite membrane prepared by the method has excellent comprehensive performance when being used for gas separation; especially, the blanded membrane filled with 1-butyl-2, 3-dimethyl imidazole hexafluorophosphate of 40% in mass percentage has high CO2 seepage velocity and CO2/CH4 and CO2/N2 selectivity, CO2 seepage coefficient in a pure gas test under a humidifying condition can reach 695 Barrer, CO2/CH4 selectivity is 35, and CO2/N4 selectivity is 42.
Description
Technical field
The present invention relates to preparation and the application of a kind of ionic liquid blend film, belong to gas membrane Seperation Technology field.
Background technology
In recent years, along with industrial expansion, combustion of fossil fuel, create a large amount of CO2Gas.It is badly in need of efficient low one-tenth at present
This carbon trapping technique.Membrane technology gets the attention due to the advantage such as green, energy consumption is low, equipment investment is low, is current
It is expected to one of technology of using on a large scale.The highest due to membrane material separating property at present, limit it and develop further.Design
Preparation tool high osmosis and the selective membrane material of height are the focuses of research at present.Conventional polymer material has good film forming
Performance and low cost feature, be the main body of membrane material.But permeability limits with the most shifting trade-off effect
The application of membrane material, is to continue to lift up permeability of the membrane and selectivity based on high molecular research.
Ionic liquid particularly ionic liquid at room temperature, due to low volatility, is a kind of material being preferably applied to carbon trapping,
Absorption field has obtained relatively broad application.Ionic liquid film is mainly prepared as supported liquid membrane at present, its mechanical stability
Poor, the most under elevated pressure conditions, ionic liquid easily runs off.Ionic liquid is blended with macromolecular material, utilizes high score
Strong and weak interaction between subchain section and particle liquid prepares membrane material, is a kind of effective method.Ionic liquid at present
Body certain applications existing with polymer blended film and gas separation field, with polyoxyethylene-polycaprolactam that filming performance is good
Block copolymer is expected to improve the stability of ionic liquid as main body.Especially for imidazole type ion liquid, be blended in
After macromolecule, the faciliated diffusion effect of imidazole group can be played under humidified condition, thus significantly improve the separating property of film.
Summary of the invention
It is an object of the invention to the preparation method and application of a kind of ionic liquid blend film.The ionic liquid prepared in this approach
Blend film is used for separating CO2/CH4、CO2/N2Mixture, has higher CO2Infiltration rate and separation factor.
The present invention propose a kind of ionic liquid blend film, key component be polyoxyethylene-polycaprolactam block copolymer and
Imidazole type ion liquid；Wherein, the mass fraction of imidazole type ion liquid is 5-50%.
Wherein, described imidazole type ion liquid is 1-butyl-2,3-methylimidazole hexafluorophosphate, 1-butyl-3 methylimidazole
In tetrafluoroborate, 1-butyl-3 methylimidazole dicyan amine salt, 1-ethyl-3-methylimidazole bis trifluoromethyl salt arbitrary containing imidazoles
Ionic liquid at room temperature.
The method preparing above-mentioned ionic liquid blend film, comprises the following steps:
Step one, by the polyoxyethylene that polyoxyethylene segment mass fraction the is 55-60%-polycaprolactam block of certain mass altogether
Polymers adds in the ethanol solution that mass fraction is 65-75%, is heated at reflux 75～90 DEG C so that it is in polyoxyethylene-poly-oneself
Lactams block copolymer is completely dissolved, and is cooled to room temperature, and prepared mass fraction is that the polyoxyethylene-polycaprolactam of 2-7% is embedding
Section copolymer solution；
Step 2, take the polyoxyethylene-polycaprolactam block copolymer solution of certain mass, be added dropwise to imidazole type ion liquid
Preparing mixed solution A, wherein, described imidazole type ion liquid accounts for the quality of polyoxyethylene-polycaprolactam block copolymer and divides
Number is 5-50%, and magnetic agitation makes imidazole type ion liquid therein be completely dissolved, and is cooled to room temperature and prepares casting solution；
Step 3, casting solution step 2 prepared add in polytetrafluoroethylene (PTFE) culture dish, and cured at room temperature film forming, in 35-60 DEG C
It is dried 24～48h under vacuum condition, obtains ionic liquid blend film.
The ionic liquid blend film of the present invention is used in gas separation, in particular for CO2/CH4Or CO2/N2Separation.
It is an advantage of the current invention that: preparation method is simple, and ionic liquid is fixed in macromolecular chain, and turnover rate is low.Obtained
Composite membrane for gas separate, have excellence combination property.Especially, use and fill 50% mass fraction 1-butyl-2,
The blend film of 3-methylimidazole hexafluorophosphate has high CO2Infiltration rate and CO2/CH4、CO2/N2Selectivity, adds
Pure gas test CO under the conditions of wet2Infiltration coefficient is up to 695Barrer, CO2/CH4Selectivity is 35, CO2/N2Selectivity is
42。
Detailed description of the invention
Being described in further detail technical solution of the present invention below in conjunction with specific embodiment, described specific embodiment is the most right
The present invention explains, not in order to limit the present invention.
Embodiment 1, the preparation of a kind of ionic liquid blend film, comprise the following steps:
Step one, to weigh 0.5g polyoxyethylene-polycaprolactam block copolymer (trade name Pebax 1657), 7g anhydrous
Ethanol and 3g deionized water, add in the there-necked flask of band condenser pipe, in the water bath with thermostatic control of 80 DEG C, with 500r/min's
Speed return stirring 2h so that it is in polyoxyethylene-polycaprolactam block copolymer all dissolve.
Step 2, weigh 0.25g 1-butyl-2,3-methylimidazole hexafluorophosphate, it is added dropwise over the polyoxy that step one prepares
In ethene-polycaprolactam block copolymer solution, with speed magnetic agitation 2h of 1000r/min, it is cooled to room temperature and prepares casting
Film liquid；
Step 3, will be poured into after casting solution standing and defoaming cleaning polytetrafluoroethylene (PTFE) culture dish (Φ 100mm) in, room temperature
Under be dried 24h film-forming, then 45 DEG C, be dried 24h under vacuum condition, obtain the ionic liquid of thickness about 100 μm
Blend film.
By above-mentioned prepared ionic liquid blend film under conditions of room temperature, test pressure are 2bar, with pure gas at humidification bar
Test under part, CO2Infiltration coefficient is 695barrer (1barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/N2
Separation factor is 42, CO2/CH4Separation factor is 35.
Embodiment 2, the preparation of a kind of ionic liquid blend film, preparation process is basically identical with embodiment 1, and difference is:
1-butyl-2 in step 2, the quality of 3-methylimidazole hexafluorophosphate is 0.025g.
Test condition is same as in Example 1, tests under humidified condition with pure gas, CO2Infiltration coefficient is 484barrer (1
Barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/N2Separation factor is 26, CO2/CH4Separation factor is 22.
Embodiment 3, the preparation of a kind of ionic liquid blend film, preparation process is basically identical with embodiment 1, and difference is:
1-butyl-2 in step 2, the quality of 3-methylimidazole hexafluorophosphate is 0.10g.
Test condition is same as in Example 1, tests under humidified condition with pure gas, CO2Infiltration coefficient is 580barrer (1
Barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/N2Separation factor is 31, CO2/CH4Separation factor is 33.
Embodiment 4, the preparation of a kind of ionic liquid blend film, preparation process is basically identical with embodiment 1, and difference is:
In step 2, imidazole type ion liquid is 1-butyl-3 methyl imidazolium tetrafluoroborate, and its quality is 0.25g.
Test condition is same as in Example 1, tests under humidified condition with pure gas, CO2Infiltration coefficient is 553barrer (1
Barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/N2Separation factor is 38, CO2/CH4Separation factor is 30.
Embodiment 5, the preparation of a kind of ionic liquid blend film, preparation process is basically identical with embodiment 1, and difference is:
In step 2, imidazole type ion liquid is 1-butyl-3 methylimidazole dicyan amine salt, and its quality is 0.25g.
Test condition is same as in Example 1, tests under humidified condition with pure gas, CO2Infiltration coefficient is 496barrer (1
Barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/N2Separation factor is 34, CO2/CH4Separation factor is 26.
Embodiment 6, the preparation of a kind of ionic liquid blend film, preparation process is basically identical with embodiment 1, and difference is:
In step 2, imidazole type ion liquid is 1-ethyl-3-methylimidazole bis trifluoromethyl salt, and its quality is 0.25g.
Test condition is same as in Example 1, tests under humidified condition with pure gas, CO2Infiltration coefficient is 633barrer (1
Barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/N2Separation factor is 29, CO2/CH4Separation factor is 24.
Comparative example 1, the preparation of a kind of hybridized film, preparation process is: weigh 0.5g polyoxyethylene-polycaprolactam block copolymerization
Thing (trade name Pebax 1657), 7g absolute ethyl alcohol and 3g deionized water, add in the there-necked flask of band condenser pipe,
In the water bath with thermostatic control of 80 DEG C, with the speed return stirring 2h of 500r/min so that it is in polyoxyethylene-polycaprolactam block
Copolymer all dissolves, and obtains casting solution, and the polytetrafluoroethylene (PTFE) being poured into cleaning after the casting solution standing and defoaming that will obtain is cultivated
In ware (Φ 100mm), under room temperature, be dried 24h, then 45 DEG C, be dried 24h under vacuum condition, obtain thickness about 100 μm
Hybridized film.
Test condition is same as in Example 1, tests under humidified condition with pure gas, CO2Infiltration coefficient is 460barrer (1
Barrer=10-10cm3(STP)cm/(cm2S cmHg)), CO2/N2Separation factor is 22, CO2/CH4Separation factor is 18.
To sum up, in preparation process of the present invention, select 1-butyl-2, ionic liquid prepared by 3-methylimidazole hexafluorophosphate
CO2Infiltration coefficient and CO2/N2, CO2/CH4Separation factor is the highest.With the increase of imidazole type ion liquid addition, CO2
Infiltration coefficient and CO2/N2, CO2/CH4Separation factor increases the most therewith.
Although above, invention has been described, but the invention is not limited in above-mentioned detailed description of the invention, above-mentioned
Detailed description of the invention is only schematic rather than restrictive, and those of ordinary skill in the art is in the enlightenment of the present invention
Under, without deviating from the spirit of the invention, it is also possible to make many variations, within these belong to the protection of the present invention.
Claims (5)
1. an ionic liquid blend film, it is characterised in that key component be polyoxyethylene-polycaprolactam block copolymer with
And imidazole type ion liquid；Wherein, the mass fraction of imidazole type ion liquid is 5-50%.
2. ionic liquid blend film as claimed in claim 1, it is characterised in that described imidazole type ion liquid is 1-butyl
-2,3-methylimidazole hexafluorophosphate, 1-butyl-3 methyl imidazolium tetrafluoroborate, 1-butyl-3 methylimidazole dicyan amine salt,
Arbitrary ionic liquid at room temperature containing imidazoles in 1-ethyl-3-methylimidazole bis trifluoromethyl salt.
3. the method preparing ionic liquid blend film as claimed in claim 1 or 2, it is characterised in that include following step
Rapid:
Step one, by the polyoxyethylene that polyoxyethylene segment mass fraction the is 55-60%-polycaprolactam block of certain mass altogether
Polymers adds in the ethanol solution that mass fraction is 65-75%, is heated at reflux 75～90 DEG C so that it is in polyoxyethylene-poly-oneself
Lactams block copolymer is completely dissolved, and is cooled to room temperature, and prepared mass fraction is that the polyoxyethylene-polycaprolactam of 2-7% is embedding
Section copolymer solution；
Step 2, take the polyoxyethylene-polycaprolactam block copolymer solution of certain mass, be added dropwise to imidazole type ion liquid
Preparing mixed solution A, wherein, described imidazole type ion liquid accounts for the quality of polyoxyethylene-polycaprolactam block copolymer and divides
Number is 5-50%, and magnetic agitation makes imidazole type ion liquid therein be completely dissolved, and is cooled to room temperature and prepares casting solution；
Step 3, casting solution step 2 prepared add in polytetrafluoroethylene (PTFE) culture dish, and cured at room temperature film forming, in 35-60 DEG C
It is dried 24～48h under vacuum condition, obtains ionic liquid blend film.
4. the application of the ionic liquid blend film that preparation method as claimed in claim 3 prepares, it is characterised in that for gas
Separate.
5. the application of ionic liquid blend film as claimed in claim 4, it is characterised in that for CO2/CH4Or CO2/N2
Separation.
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| CN201610235201.9A CN105749769B (en) | 2016-04-13 | 2016-04-13 | A kind of preparation and application of ionic liquid blend film |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107694353A (en) * | 2017-09-05 | 2018-02-16 | 齐齐哈尔大学 | The preparation method of ethyl cellulose and ionic liquid gas separation membrane |
| CN110404424A (en) * | 2019-06-17 | 2019-11-05 | 沈阳工业大学 | Mixed substrate membrane containing nano-grade molecular sieve and preparation method and applications |
| CN111467933A (en) * | 2019-01-23 | 2020-07-31 | 中国科学院过程工程研究所 | Method for selectively separating ammonia gas by multi-site proton type ionic liquid composite membrane |
| CN111804161A (en) * | 2019-04-12 | 2020-10-23 | 天津工业大学 | For CO2Separated amino acid ion liquid coated nano microsphere/polymer hybrid membrane |
| CN112973468A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for preparing two-dimensional covalent organic framework ultrathin nanosheet material composite membrane and application |
| CN113457469A (en) * | 2021-08-04 | 2021-10-01 | 中国矿业大学 | High-temperature-resistant PDMS/ionic liquid composite membrane and preparation method and application thereof |
| CN114425246A (en) * | 2020-09-28 | 2022-05-03 | 中国石油化工股份有限公司 | Ionic liquid supported composite membrane and preparation method and application thereof |
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| CN103521100A (en) * | 2013-10-29 | 2014-01-22 | 天津大学 | High-molecular-functional mesoporous silica hybrid membrane, preparation method and applications |
| CN103894081A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | Cross-linked polyoxyethylene-polycaprolactam block copolymer film as well as preparation and application thereof |
| CN104741009A (en) * | 2015-03-20 | 2015-07-01 | 江苏大学 | Preparation method of salicylic acid molecular imprinted cellulose acetate blended membrane and application of blended membrane |
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| US20120302678A1 (en) * | 2010-01-18 | 2012-11-29 | Korea Institute Of Energy Research | Ionic liquid-polymer gel membrane with improved gas permeability, and preparation method thereof |
| CN103521100A (en) * | 2013-10-29 | 2014-01-22 | 天津大学 | High-molecular-functional mesoporous silica hybrid membrane, preparation method and applications |
| CN103894081A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | Cross-linked polyoxyethylene-polycaprolactam block copolymer film as well as preparation and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107694353A (en) * | 2017-09-05 | 2018-02-16 | 齐齐哈尔大学 | The preparation method of ethyl cellulose and ionic liquid gas separation membrane |
| CN111467933B (en) * | 2019-01-23 | 2021-09-07 | 中国科学院过程工程研究所 | Method for selectively separating ammonia gas by multi-site proton type ionic liquid composite membrane |
| CN111467933A (en) * | 2019-01-23 | 2020-07-31 | 中国科学院过程工程研究所 | Method for selectively separating ammonia gas by multi-site proton type ionic liquid composite membrane |
| CN111804161A (en) * | 2019-04-12 | 2020-10-23 | 天津工业大学 | For CO2Separated amino acid ion liquid coated nano microsphere/polymer hybrid membrane |
| CN110404425A (en) * | 2019-06-17 | 2019-11-05 | 沈阳工业大学 | Graft type ionic liquid polyimide film and preparation method and applications |
| CN110404424A (en) * | 2019-06-17 | 2019-11-05 | 沈阳工业大学 | Mixed substrate membrane containing nano-grade molecular sieve and preparation method and applications |
| CN110404425B (en) * | 2019-06-17 | 2021-11-23 | 沈阳工业大学 | Grafted ionic liquid polyimide membrane, preparation method and application thereof |
| CN110404424B (en) * | 2019-06-17 | 2021-12-14 | 沈阳工业大学 | Mixed matrix membrane and preparation method and application thereof |
| CN112973468A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for preparing two-dimensional covalent organic framework ultrathin nanosheet material composite membrane and application |
| CN112973468B (en) * | 2019-12-14 | 2022-04-08 | 中国科学院大连化学物理研究所 | Method for preparing two-dimensional covalent organic framework ultrathin nanosheet material composite membrane and application |
| CN114425246A (en) * | 2020-09-28 | 2022-05-03 | 中国石油化工股份有限公司 | Ionic liquid supported composite membrane and preparation method and application thereof |
| CN114425246B (en) * | 2020-09-28 | 2023-04-11 | 中国石油化工股份有限公司 | Ionic liquid supported composite membrane and preparation method and application thereof |
| CN113457469A (en) * | 2021-08-04 | 2021-10-01 | 中国矿业大学 | High-temperature-resistant PDMS/ionic liquid composite membrane and preparation method and application thereof |
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Granted publication date: 20190111 |