CN106823849B - Ultra-thin zeolite imidazole ester skeleton hybridized film, preparation method and application - Google Patents
Ultra-thin zeolite imidazole ester skeleton hybridized film, preparation method and application Download PDFInfo
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- CN106823849B CN106823849B CN201510886177.0A CN201510886177A CN106823849B CN 106823849 B CN106823849 B CN 106823849B CN 201510886177 A CN201510886177 A CN 201510886177A CN 106823849 B CN106823849 B CN 106823849B
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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
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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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/46—Impregnation
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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
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- 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
Abstract
Ultra-thin zeolite imidazole ester skeleton hybridized film, preparation method and application, the hybridized film are dispersed in organic solvent using ultra-thin zeolite imidazole ester skeleton nanometer sheet, are first formed a film in carrier surface, then polymer film forming is carried out 1~10 formation hybridized film on it.Zeolite imidazole ester skeleton nanometer sheet and organic polymer have good interface compatibility in zeolite imidazole ester skeleton hybridized film prepared by the present invention, therefore have good gas separating property.Synthetic method of the invention is simple, reproducible, can be applied to various complex carriers.
Description
Technical field
The invention belongs to UF membrane fields, and in particular to a kind of ultra-thin zeolite imidazole ester skeleton hybridized film is synthesized and answered
With.
Background technique
Energy-conserving and emission-cutting technology is the key that realize one of sustainable development, environmental-friendly.It is total that separation process accounts for process industrial
The 40%~60% of energy consumption, thus the energy-saving and emission-reduction of separation process become global researcher pay close attention to object it
One.UF membrane has that low energy consumption, and separative efficiency is high, easy to operate, the significant advantages such as low-carbon emission, can be employed for gas point
From, sea water desalination, in the numerous areas such as water pollution control and pharmacy.Gas separation membrane market mainly accounts for master by polymer film at present
Lead status, but its thermal stability and chemical stability be not high, in addition, so far polymer film gas separating property because
" trade-off " effect is respectively positioned on Robinson's upper limit (Robeson ' s upper bound) below.
Organic-inorganic hybrid films are one of solutions, combine inorganic filler (such as highly selective) with it is organic
The advantages of both polymer (such as high penetration), large scale preparation can be realized using existing technology.Common inorganic fill
Grain such as zeolite molecular sieve, silica, carbon molecular sieve, because with polymer incompatibility, obtained hybridized film often there are
Two-phase gap, causes film properties to decline.
Metal organic framework is the ordered crystal structure formed by metal ion and organic ligand by coordination, due to
The presence of organic ligand, usual this kind of material and polymer have good interface compatibility, can overcome traditional inorganic fill material
The problems such as the shortcomings that material, is with the plasticizing of neat polymer film, aging.However hydridization film thickness in general sense is substantially in the micron-scale
More than, membrance permeability amount is low, it is difficult to meet industrialization demand.Use metal organic framework nanometer sheet material as filler, then may
The hybridized film of ultrathin is prepared, membrance permeability amount can be significantly greatly increased in extremely short gas molecule transmission path, be expected to be applied to more
Kind industrial gasses separation field.We formerly study the technology that disclosed ball milling adds ultrasonic layers apart two-dimensional layer persursor material
(201410714849.5) a large amount of complete zeolite imidazole ester skeleton nanometer sheets can be obtained, this nanometer sheet thickness is no more than 100
Nanometer, is the construction unit of very ideal high penetration hybridized film.
Summary of the invention
To solve organic-inorganic hybrid films in the prior art there are inorganic material and organic matter poor compatibility, cause to prepare
Hybridized film have a two-phase gap, the problem of film properties difference, the present invention draws up a kind of standby ultra-thin zeolite imidazole ester skeleton hybridized film.
To realize that the above technical purpose, the present invention disclose a kind of preparation side of ultra-thin zeolite imidazole ester skeleton hybridized film first
Method includes the following steps:
1. preparation of nano piece dispersion liquid: zeolite imidazole ester skeleton nanometer sheet being placed in organic solvent I and forms nanometer sheet point
Dispersion liquid, in dispersion liquid, the zeolite imidazole ester skeleton nanometer sheet is calculated as 0.01~0.1mg/mL with concentration；
2. prepared polymer solution: polymer is mixed with organic solvent II and is made into polymer solution, wherein polymer with
Score is calculated as 0.01%~15%；
The polymer is selected from poly [2,2 '-(p-oxydiphenylene) -5,5 '-bibenzimidazole]
(OPBI), one of polybenzimidazoles, polyimides and polysulfones；
3. forming a film in porous carrier surface: nanometer sheet dispersion liquid first being dropped to porous carrier surface, stands or drying is formed
Nanometer sheet film；Again in the surface coated polymer solution of nanometer sheet film, polymer film is formed, it is dry, form Double-layer clamp film；
4. the operation of step 3. is carried out 1~10 time, the ultra-thin zeolite imidazole ester skeleton hybridized film is obtained.
It should be noted that in the above preparation method, the zeolite imidazole ester skeleton nanometer sheet uses
Method preparation in CN201410714849.5: after two-dimensional metallic organic framework material is mixed with organic solvent, wet ball grinding
Processing, obtains required zeolite imidazole ester skeleton nanometer sheet；As a further preference, the zeolite imidazole ester skeleton nanometer is prepared
When piece, the two-dimensional metallic organic framework material used is Zn2(bim)4Or Zn2(bim)3, wherein bim is benzimidazole.
Further, in the above preparation method, step 2. described in polymer solution concentration be 0.02~1.5%；
Step 3. in the mode of polymer film forming be that dip-coating method form a film or directly drop to carrier or nanometer sheet film surface forms a film；When with
When directly dropping to carrier or nanometer sheet film surface film forming, the dripping quantity of the polymer solution is 0.005~0.08mL/cm2It carries
Body, preferably 0.007~0.04mL/cm2Carrier.
Further, in order to preferably form a film and increase the compatibility between nanometer sheet film and polymer film, step 3. in
When preparing nanometer sheet film, in terms of the carrier of unit area, the dripping quantity of the nanometer sheet dispersion liquid is 0.3~24mL/cm2It carries
Body.
Further, it will be apparent to a skilled person that step 4. in, it is described to carry out step operation 3.
1~10 time, the hybridized film of nanometer sheet film and polymer film alternately superposition can be prepared, on microcosmic, the hybridized film has 2~
20 film structures.Preferably, the operation of step 3. is carried out 1~3 time.
Further, the organic solvent I is in methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol and isobutanol
At least one, the organic solvent II are selected from n,N-dimethylacetamide, n,N-Dimethylformamide, chloroform, N- methylpyrrole
At least one of alkanone and tetrahydrofuran.
Further, it will be apparent to a skilled person that the porous carrier is carrier commonly used in the art, make
To be preferred, the shape of the porous carrier is sheet, and netted or tubulose is carried selected from alumina support, titanium dioxide carrier, stainless steel
Body, polypropylene carrier, polysulfone support, Kynoar carrier, Haloport F, polyethersulfone support and polyacrylonitrile carrier
One of.
Another technical purpose of the invention is to provide the ultra-thin zeolite imidazole ester prepared by made as described above method
Skeleton hybridized film.Hybridized film prepared by the present invention is alternately formed by stacking by nanometer sheet film and polymer film, phase between two kinds of ingredients
Capacitive is preferable, and separating property is excellent.
Compared with prior art, the invention has the following advantages that
Packing material of the present invention using zeolite imidazole ester skeleton nanometer sheet as organic film, instead of traditional inorganic material,
Ultra-thin zeolite imidazole ester skeleton hybridized film is prepared, this zeolite imidazole ester skeleton nanometer sheet and organic polymer have good interface
Compatibility has good gas separating property.And synthetic method of the invention is simple, reproducible, synthetic method can answer
For various complex carriers.
Detailed description of the invention
Fig. 1 is the I surface Scanning Electron microscope photo of hybridized film that embodiment 1 synthesizes；
Fig. 2 is the I cross sectional scanning electron microscope photo of hybridized film that embodiment 1 synthesizes；
Fig. 3 is the x-ray diffraction pattern for the hybridized film I that embodiment 1 synthesizes；
Fig. 4 is the x-ray diffraction pattern for the hybridized film II that embodiment 4 synthesizes.
Specific embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.
Zn used in the embodiment of the present invention2(bim)4Nanometer sheet and Zn2(bim)3Nanometer sheet is respectively adopted
The method preparation of specific embodiment part embodiment 2~5 in CN201410714849.5.
Embodiment 1
Zn2(bim)4The preparation of nanometer sheet@OPBI hybridized film I:
1. by Zn2(bim)4Nanometer sheet, which is scattered in methanol, forms dispersion liquid, Zn2(bim)4Nanometer sheet concentration is 0.04mg/
mL。
2. OPBI is dissolved in n,N-dimethylacetamide, compound concentration is the polymer solution of 0.05wt%.
③α-Al2O3Porous carrier is placed on 120 DEG C of heating platforms, by Zn2(bim)4Nanometer sheet/methanol dispersion liquid is dropwise
It drips in its surface (with 5.9mL dispersion liquid/cm2Carrier meter), it is 1 hour dry.
4. carrier is transferred on room temperature platform, dropwise be added dropwise OPBI polymer solution (with 0.024mL polymer solution/
cm2Carrier meter), it is one hour dry at 70 DEG C,
5. repeatedly 3., 4. step 2 time drop piece is film-made.
Electron scanning micrograph (Fig. 1) shows that polymeric layer is very thin, can clearly see nanometer sheet pattern clearly.It cuts
The scanning electron microscope microscope photo in face shows that (Fig. 2) shows that film thickness is about 50 nanometers.X-ray diffraction spectrogram (Fig. 3) is located at
There is a bulge peak near 12 °, illustrate that nanometer sheet along the unordered stacking in vertical carrier direction, exposes duct as much as possible,
Therefore hydrogen penetration is big, and separation is high, after cover aggregation object, still maintains the good pattern of nanometer sheet, 25 ° of later peaks are
α-Al2O3The characteristic peak of carrier.
Embodiment 2-3
According to identical method in embodiment 1, two duplicate parallel laboratory tests have been carried out, have separately been prepared for two Zn2(bim)4
Nanometer sheet@OPBI hybridized film, number is hybridized film I and hybridized film II and hybridized film III respectively.
Embodiment 4
Zn2(bim)4The preparation of nanometer sheet@OPBI hybridized film II
1. by Zn2(bim)4Nanometer sheet, which is scattered in methanol, forms dispersion liquid, Zn2(bim)4Nanometer sheet concentration is 0.04mg/
mL。
2. OPBI is dissolved in n,N-dimethylacetamide, compound concentration is the polymer solution of 0.02wt%.
3. by Zn2(bim)4Nanometer sheet/methanol dispersion liquid is dripped dropwise at 120 DEG C in α-Al2O3Porous carrier surface (with
5.9mL dispersion liquid/cm2Carrier meter), it is 12 hours dry at 60 DEG C, it is 12 hours dry under 60 DEG C of vacuum.
4. thering is the alumina carrier surface of nanometer sheet to lift a thin layer polymer solution in load using dip-coating method, mention
Draw parameter are as follows: upstream rate: 20mm/min, downstream rate: 60mm/min, stop: 10 seconds, lift number: 1 time, with caudacoria in
It dries 48 hours at room temperature, is transferred at 70 DEG C of oven dryings 12 hours, 150 DEG C 12 hours dry, drying 12 under 150 DEG C of vacuum
Hour.
X-ray diffraction spectrogram (Fig. 4) is located at the characteristic peak that the peak near 9 ° is nanometer sheet, equally illustrates that the hybridized film is poly-
It is very thin to close nitride layer, 25 ° of later peaks are α-Al2O3The characteristic peak of carrier.
Embodiment 5
Zn2(bim)3The preparation of nanometer sheet@OPBI hybridized film IV:
Except step 1. in Zn2(bim)3Nanometer sheet replaces Zn2(bim)4Nanometer sheet, the solvent for dispersing nanometer sheet select first
Outside the mixed liquor of pure and mild normal propyl alcohol, other are the same as embodiment 1.
Comparative example 1
Step and material first prepare polymer film unlike the first embodiment with embodiment 1 on carrier, then on it
Nanometer sheet film is prepared, i.e., prepares hybridized film a according to sequence 1., 2., 4., 3..
The measurement of hybridized film gas separating property:
The silicagel pad for having 5 mm dia apertures and stainless steel wafer are carefully covered on to the hydridization of the preparation of embodiment 1,2
Film is encapsulated in Brunswick-Callenbach (Wicke-Kallenbach) membrane module, in the item of room temperature and △ P=0 bar by film surface
Under part, hydrogen/carbon dioxide gas mixture separation test is carried out, argon gas is as purge gass.Test the gas separation of different films
Performance, all results are as shown in the table:
Thus table is as it can be seen that using Zn prepared by the present invention2(bim)4Nanometer sheet@OPBI hybridized film not only gas separating property
Height, and it is reproducible.And there have the gas separating property result of the hybridized film a of the preparation of comparative example 1 can be seen that be miscellaneous when that will prepare
When changing the sequence of nanometer sheet film and polymer film exchange in film, the hybridized film of preparation does not have the energy of separation hydrogen and carbon dioxide
Power.
Claims (11)
1. the preparation method of ultra-thin zeolite imidazole ester skeleton hybridized film, includes the following steps:
1. preparation of nano piece dispersion liquid: zeolite imidazole ester skeleton nanometer sheet is placed in organic solvent I and forms nanometer sheet dispersion liquid,
In dispersion liquid, the zeolite imidazole ester skeleton nanometer sheet is calculated as 0.01~0.1mg/mL with concentration；
2. prepared polymer solution: polymer being mixed with organic solvent II and is made into polymer solution, wherein polymer is with quality
Score is calculated as 0.01~15%；
The polymer is selected from OPBI (poly [2,2 '-(p-oxydiphenylene) -5,5 '-bibenzimidazole]), gathers
One of benzimidazole, polyimides and polysulfones；
3. forming a film in porous carrier surface: nanometer sheet dispersion liquid first being dropped to porous carrier surface, stands or drying forms nanometer
Piece film；Again in the surface coated polymer solution of nanometer sheet film, polymer film is formed, it is dry, form Double-layer clamp film；
4. the operation of step 3. is carried out 1~10 time, the ultra-thin zeolite imidazole ester skeleton hybridized film is obtained.
2. preparation method according to claim 1, which is characterized in that 3. the middle mode for forming polymer film is dipping to step
Czochralski method film forming directly drops to carrier or nanometer sheet film surface film forming.
3. preparation method according to claim 1, which is characterized in that step 2. described in polymer solution concentration with matter
Amount score is calculated as 0.02~1.5%.
4. preparation method according to claim 3, which is characterized in that the mode of the polymer solution film forming is directly to drip
When to nanometer sheet film surface film forming, in terms of the carrier of unit area, the dripping quantity of the polymer solution is 0.005~
0.08mL/cm2Carrier.
5. preparation method according to claim 1, which is characterized in that step 3. in preparation nanometer sheet film when, with unit plane
Long-pending carrier meter, the dripping quantity of the nanometer sheet dispersion liquid are 0.3~24mL/cm2Carrier.
6. preparation method according to claim 5, which is characterized in that step 3. in preparation nanometer sheet film when, with unit plane
Long-pending carrier meter, the dripping quantity of the nanometer sheet dispersion liquid are 5~18mL/cm2Carrier.
7. preparation method according to claim 1, which is characterized in that the organic solvent I is selected from methanol, ethyl alcohol, positive third
At least one of alcohol, isopropanol, n-butanol and isobutanol.
8. preparation method according to claim 1, which is characterized in that the organic solvent II is selected from N, N- dimethylacetamide
At least one of amine, N,N-dimethylformamide, chloroform, N-Methyl pyrrolidone and tetrahydrofuran.
9. preparation method according to claim 1, which is characterized in that the zeolite imidazole ester skeleton hybridized film is using following
Step preparation:
1. taking Zn2(bim)4Or Zn2(bim)3Nanometer sheet is placed in organic solvent I and forms Zn2(bim)4Or Zn2(bim)3Nanometer sheet
The dispersion liquid of 0.015~0.04mg/mL is calculated as with concentration；
2. it is 0.02~1.5% that polymer OPBI is dissolved in DMAC N,N' dimethyl acetamide to form polymer based on mass fraction；
3. nanometer sheet dispersion liquid is first dropped into porous carrier surface in porous carrier surface, stand or drying and forming-film after, then in table
Face coated polymer solution film forming, in terms of the carrier of unit area, the dripping quantity of nanometer sheet dispersion liquid and polymer solution is distinguished
For 5~18mL/cm2Carrier and 0.007~0.04mL/cm2Carrier；
4. the operation of step 3. is carried out 1~3 time, the ultra-thin zeolite imidazole ester skeleton hybridized film is obtained.
10. the ultra-thin zeolite imidazole ester skeleton hybridized film of preparation method preparation described in any one of claim 1 to 9.
11. ultra-thin zeolite imidazole ester skeleton hybridized film described in any one of claim 10 is in separation CO2In application.
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| CN109233274B (en) * | 2018-09-13 | 2020-12-15 | 吉林大学 | Polybenzimidazole membrane with nano porous structure and preparation method thereof |
| CN111249917B (en) * | 2018-11-30 | 2021-10-26 | 中国科学院大连化学物理研究所 | Preparation method and application of SAPO-34 based mixed matrix membrane |
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| US5091087A (en) * | 1990-06-25 | 1992-02-25 | Hoechst Celanese Corp. | Fabrication of microporous PBI membranes with narrow pore size distribution |
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