CN105879704A - Preparation method and application of mixed matrix membrane containing zeolite imidazolate framework material - Google Patents
Preparation method and application of mixed matrix membrane containing zeolite imidazolate framework material Download PDFInfo
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- CN105879704A CN105879704A CN201610176131.4A CN201610176131A CN105879704A CN 105879704 A CN105879704 A CN 105879704A CN 201610176131 A CN201610176131 A CN 201610176131A CN 105879704 A CN105879704 A CN 105879704A
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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
- B01D69/14—Dynamic membranes
- B01D69/141—Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes
- B01D69/148—Organic/inorganic mixed matrix membranes
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D71/02—Inorganic material
- B01D71/028—Molecular sieves
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/501—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
- C01B3/503—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion characterised by the membrane
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/0475—Composition of the impurity the impurity being carbon dioxide
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a preparation method and application of a mixed matrix membrane prepared by compositing a zeolite imidazolate framework material (ZIF hereafter represents the zeolite imidazolate framework material for the sake of narration) ZIF-7 with Matrimid polymide, and belongs to the technical field of membrane separation. The membrane is the mixed matrix membrane of ZIF-7 and Matrimid polymide (the chemical name is 5(6)-amino-1-(4'-aminophenyl)-1,3-trimethyl indene alkane, the trade name is Matrimid-5218, and Matrimid hereafter represents Matrimid polymide for the sake of narration), that is, the ZIF-7-Matrimide membrane and is used for separation of H2-CO2 mixed gas. The preparation method has the advantages that the preparation cost of ZIF-7 is lower than that of many MOF materials; the ZIF-7-Matrimid membrane combines the advantages of the zeolite imidazolate framework material ZIF-7 with the advantages of the polymer material Matrimid, and compared with a pure Matrimid membrane, the ZIF-7-Matrimid membrane has the advantages that the permeability is greatly improved, and the high selectivity is kept; the membrane shows the very good separation effect on the H2-CO2 mixed gas and has the huge application value in the fields of water gas hydrogen production.
Description
Technical field
The present invention relates to membrance separation field, a kind of ZIF-7/ that gas is isolated and purified in chemical industry
The preparation method and applications of Matrimid mixed substrate membrane containing nano-grade molecular sieve.
Background technology
Hydrogen, as a kind of novel and energy of cleaning, provides new solution to the problem such as environment, the energy.Currently
One of large-scale production main path of hydrogen is water gas method hydrogen manufacturing, and the primary product of this method is hydrogen and carbon dioxide.
Conventional hydrogen method of purification is solution absorption method, and this method equipment is complicated, comprehends and produce certain environmental effect at solution.Use film
The mode separated, equipment is simple, and energy-conserving and environment-protective, cost is relatively low simultaneously.
Gaseous jet simulation is a kind of green continuable isolation technics.Compared to traditional pressure-variable adsorption and cryogenic rectification etc.
Method, membrance separation has low energy consumption, pollution-free, free from admixture introduces, process equipment is simple, safety advantages of higher.Gas separates
Film is broadly divided into organic high molecular layer and inoranic membrane, the former mainly utilize the dissolving-diffusibility different in film of gas and will be mixed
Conjunction gas separates, and the latter mainly separates mixed gas by absorption with the principle such as shape-selective screening.Two kinds of films are respectively arranged with pluses and minuses.Nothing
Machine film is rigid film, has the strongest molecule sieving capacity, but the film forming of being difficult to and fragility are relatively big, and the life-span is short；Organic membrane is just
On the contrary, gas permeation ability is more weak, and selectivity and permeability are conflicting, and the Robeson upper limit i.e. characterizes selectivity and infiltration
The feature that mutually restricts of property.Advantage is then to prepare simply, it is easy to film forming, is the main body of current membrance separation industry.
Mixed substrate membrane containing nano-grade molecular sieve (Mixed Matrix Membranes) is a kind of inorganic material to be mixed in organic substrate uniformly
Film prepared by mixing.It can integrate inoranic membrane and organic membrane advantage, to break through the contradiction of the selection of organic membrane-pass through
Property, surmount the Robeson upper limit, thus realize the separation purpose with higher gas selective penetrated property.Different inorganic-organic materials
Mixed substrate membrane containing nano-grade molecular sieve prepared by material combination can be used for different mixing gas system and separates, and the suitability is wide, preparation simplicity, has potential
Prospects for commercial application.
Metal organic frame (Metal-Organic Frameworks, MOFs) material is mainly by units such as oxygen-containing, nitrogen
The multiple tooth organic ligand of element is coordinated, with transition metal ions, one-dimensional, the two-dimentional or three dimensional periodic structure material assembled.Mesh
Before synthesized thousands of kinds of MOFs materials.It has a big specific surface area, higher porosity, flexible adjustable pore structure, and
Framing structure and material property can be regulated, at field tools such as separation, catalysis, pharmacy, the absorption of gas and storages by modification
Be widely used space.
Class zeolite imidazole framework (Zeolitic Imidazolate Frameworks, ZIFs) material is that a class is with imidazoles
Or imidazoles substituent is the MOFs material that part is formed with transition metal ions coordination.Except possessing the premium properties of MOFs material
Outward, ZIFs material has the Some features of molecular sieve concurrently, thus has higher chemical stability and heat stability.ZIF-7 is one
Planting the material with sodalite structure, aperture is highly uniform, about 0.3 nm.There are some researches show ZIF-7 film to H2/CO2System has
There is higher separating property.
Inventive film is mixed substrate membrane containing nano-grade molecular sieve based on ZIF-7 Yu Matrimid, i.e. ZIF-7/Matrimid film has ZIF-concurrently
The advantage of 7 and Matrimid, has excellent gas separating property.In inventive film, ZIF-7 granule is uniformly dispersed, with
Matrimid has the good compatibility.The feeding gas of inventive film is H2/CO2Mixed gas, at room temperature by dissolving-expanding
Dissipate and molecule screening realizes separating.
Summary of the invention
It is an object of the invention to provide one by class zeolite imidazole frame material ZIF-7 and polyimides Matrimid group
The preparation method and applications of mixed substrate membrane containing nano-grade molecular sieve closed, it is characterised in that there is following preparation process and step:
The preparation of a, ZIF-7 nano-particle is by 0.265 g zinc chloride (ZnCl2) and 0.310 g benzimidazole be dissolved in 30 ml
In N-N dimethylformamide (DMF), add 0.465 g diethylamine, stir about 30 minutes, pour reactor into, anti-at 130 DEG C
Answer 24 hours.After reaction terminates, centrifugal product of collecting, methanol cleaning 3 times is also centrifuged, is placed on drying overnight in 60 DEG C of baking ovens；
B, the preparation of pure Matrimid preparation liquid uses the polyimides of the entitled Matrimid in commercial goods 5218 to be raw material system
Standby required preparation liquid；By 0.40 g Matrimid batch dissolution in chloroform, stir 48 hours to obtain uniform masking
Liquid；Ultrasonic and stir；Stand and prepare knifing；
C, it is 5 ~ 30 wt% that ZIF-7 weight/mass percentage composition is prepared in the preparation of mixed substrate membrane containing nano-grade molecular sieve preparation liquid, corresponding Matrimid mass
Percentage composition be 95 ~ 70 wt% mixed substrate membrane containing nano-grade molecular sieve needed for preparation liquid；The ZIF-7 nano-particle of respective quality is dispersed in trichlorine
In methane, within ultrasonic 30 minutes, ZIF-7 granule is made to be uniformly dispersed；It is dividedly in some parts the Matrimid of respective quality the most wherein, stirs
Mix 48 hours to obtain uniform preparation liquid；Before knifing ultrasonic and stir；Stand and prepare knifing；
D, plate glass and blade applicator are asked wash clean, are uniformly poured on plate glass by preparation liquid by masking, use blade applicator to exist
Carry out knifing on plate glass, taken off after film is dry at once, put in baking oven and anneal 16 hours at 180 DEG C；Final prepared
Mixed substrate membrane containing nano-grade molecular sieve.
Matrimid polyimides used in invention, entitled 5 (6)-amino-1-(4 '-aminophenyl)-1,3-of its chemistry
Trimethyl indenes alkane, trade name Matrimid 5218.
After preparation ZIF-7/Matrimid film, also inventive film is carried out sign and performance detection.
Class zeolite imidazole frame material mixed substrate membrane containing nano-grade molecular sieve of the present invention can be used for gas membrane Seperation Technology, is applied to H2/
CO2Mixed gas separates.
Compared with prior art, the invention has the beneficial effects as follows: use prepared by ZIF-7 nano-particle and Matrimid
Mixed substrate membrane containing nano-grade molecular sieve compact structure, ZIF-7 granule is uniformly dispersed；Compared to other MOFs materials, ZIF-7 preparation cost is the lowest
Honest and clean, stable performance, be suitable to commercial Application；Inventive film has the advantage of MOFs film and organic membrane concurrently, has higher separation and passes through
Performance；Compared to traditional separate mode, membrane separation technique has low energy consumption, pollution-free, free from admixture introduces, process equipment letter
Single, safety advantages of higher.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) photo, wherein (a) ZIF-7 particle surface figure；(b) ZIF-7/
The sectional view of Matrimid film.
Fig. 2 is X-ray diffraction (XRD) figure: ZIF-7 nano-particle in (a) embodiment of the present invention；(b) ZIF-7/
Matrimid film；(c) Matrimid film.
Fig. 3 is ZIF-7/Matrimid film gas separation effect figure of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment, the present invention is further elaborated.
Embodiment 1
The preparation of ZIF-7/Matrimid mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps:
The preparation of 1.ZIF-7 nano-particle: by 0.265 g zinc chloride (ZnCl2) and 0.310 g benzimidazole be dissolved in 30 ml
In N-N dimethylformamide (DMF), add 0.465 g diethylamine, stir about 30 minutes, pour reactor into, anti-at 130 DEG C
Answer 24 hours.After reaction terminates, centrifugal product of collecting, methanol cleaning 3 times is also centrifuged, is placed on drying overnight in 60 DEG C of baking ovens.
2. the preparation of preparation liquid: prepare preparation liquid needed for the mixed substrate membrane containing nano-grade molecular sieve that weight/mass percentage composition is 5 wt%.By 0.02 g
ZIF-7 nano-particle is dispersed in chloroform, within ultrasonic 30 minutes, makes ZIF-7 granule be uniformly dispersed.It is dividedly in some parts wherein
0.38 g Matrimid, stirs 48 hours to obtain uniform preparation liquid.Before knifing ultrasonic and stir, stand and prepare knifing.
3. masking: plate glass and blade applicator are asked wash clean, is uniformly poured on preparation liquid on plate glass, uses knifing
Device carries out knifing on plate glass, is taken off at once, put in baking oven and anneal 16 hours at 180 DEG C after film is dry；Finally
Prepare mixed substrate membrane containing nano-grade molecular sieve.
Embodiment 2
The preparation of ZIF-7/Matrimid mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps:
The preparation of 1.ZIF-7 nano-particle
With above-described embodiment 1.
2. the preparation of preparation liquid: prepare preparation liquid needed for the mixed substrate membrane containing nano-grade molecular sieve that weight/mass percentage composition is 10 wt%.By 0.04
G ZIF-7 nano-particle is dispersed in chloroform, within ultrasonic 30 minutes, makes ZIF-7 granule be uniformly dispersed.It is dividedly in some parts wherein
0.36 g Matrimid, stirs 48 hours to obtain uniform preparation liquid.Before knifing ultrasonic and stir, stand and prepare knifing.
3. masking
With above-described embodiment 1.
Embodiment 3
The preparation of ZIF-7/Matrimid mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps:
The preparation of 1.ZIF-7 nano-particle
The same embodiment 1.
2. the preparation of preparation liquid: prepare preparation liquid needed for the mixed substrate membrane containing nano-grade molecular sieve that weight/mass percentage composition is 20 wt%.By 0.08
G ZIF-7 nano-particle is dispersed in chloroform, within ultrasonic 30 minutes, makes ZIF-7 granule be uniformly dispersed.It is dividedly in some parts wherein
0.32 g Matrimid, stirs 48 hours to obtain uniform preparation liquid.Before knifing ultrasonic and stir, stand and prepare knifing.
3. masking
The same embodiment 1.
Embodiment 4
The preparation of ZIF-7/Matrimid mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps:
The preparation of 1.ZIF-7 nano-particle
The same embodiment 1.
2. the preparation of preparation liquid: prepare preparation liquid needed for the mixed substrate membrane containing nano-grade molecular sieve that weight/mass percentage composition is 30 wt%.By 0.12
G ZIF-7 nano-particle is dispersed in chloroform, within ultrasonic 30 minutes, makes ZIF-7 granule be uniformly dispersed.It is dividedly in some parts wherein
0.28 g Matrimid, stirs 48 hours to obtain uniform preparation liquid.Before knifing ultrasonic and stir, stand and prepare knifing.
3. masking
The same embodiment 1.
Comparative example
The preparation of pure Matrimid film:
1. the preparation of preparation liquid: prepare preparation liquid needed for pure Matrimid film.By 0.40 g Matrimid batch dissolution in trichlorine
In methane, stir 48 hours to obtain uniform preparation liquid.Before knifing ultrasonic and stir, stand and prepare knifing.
2. masking
The same embodiment 1.
Explanation to accompanying drawing
Fig. 1 is scanning electron microscope (SEM) photo, wherein (a) ZIF-7 particle surface figure；(b) ZIF-7/Matrimid film
Sectional view.Figure (a) is it can be seen that ZIF-7 particle size is 10 nm* (300-500) nm.This is can be seen that by figure (b)
The ZIF-7/Matrimid film even compact of bright preparation, ZIF-7 nano-particle good dispersion in film, have very with Matrimid
The good compatibility.
Fig. 2 is X-ray diffraction (XRD) figure: ZIF-7 nano-particle prepared by (a) embodiment of the present invention；(b) ZIF-7/
Matrimid film；(c) Matrimid film.In figure, the diffraction maximum of visible ZIF-7/Matrimid film of the present invention has ZIF-7 granule concurrently
Characteristic peak and the amorphous peak of Matrimid polymer, illustrate in mixed substrate membrane containing nano-grade molecular sieve biphase compound good.
Fig. 3 is ZIF-7/Matrimid film gas separation effect figure of the present invention.Mix the mixed substrate membrane containing nano-grade molecular sieve of ZIF-7 as seen from the figure
Compared with pure Matrimid film, H2Penetration and H2/CO2Ideal separation factor all increased.ZIF-7/Matrimid mixed base
Plasma membrane passes through H2Ability strengthen, H along with the increase of ZIF-7 content2/CO2Ideal separation factor then present and first increase to
The trend that then figure of merit reduces.The embodiment of optimum quality percentage composition 10 % is than the pure film H of comparative examples 52Penetration increases
36.7 %, ideal separation factor increases by 14.9 % on year-on-year basis, it is achieved that good gas separating property.
Following table table 1 is above-described embodiment ZIF-7/Matrimid mixed substrate membrane containing nano-grade molecular sieve and the test result of pure Matrimid film.
。
Claims (1)
1. the system of the mixed substrate membrane containing nano-grade molecular sieve combined with polyimides Matrimid by class zeolite imidazole frame material ZIF-7
Preparation Method, it is characterised in that there is following preparation process and step:
A. the preparation of class zeolite imidazole frame material ZIF-7 nano-particle is by 0.265 g zinc chloride (ZnCl2) and 0.310 g benzene
And imidazoles is dissolved in 30 ml N-N dimethylformamide (DMF), adds 0.465 g diethylamine, stir about 30 minutes, pour into
Reactor, reacts 24 hours at 130 DEG C；After reaction terminates, centrifugal product of collecting, methanol cleaning 3 times is also centrifuged, then puts
Drying overnight in 60 DEG C of baking ovens；
The preparation of the purest Matrimid preparation liquid uses the polyimides of the entitled Matrimid in commercial goods 5218 to be raw material
Prepare preparation liquid needed for pure Matrimid film, by 0.28 g Matrimid batch dissolution in chloroform, stir 48 hours with
Obtain uniform preparation liquid, ultrasonic and stir；Stand and prepare knifing；
C. ZIF-7 weight/mass percentage composition is prepared in the preparation of mixed substrate membrane containing nano-grade molecular sieve preparation liquid is 5 ~ 30 wt%, corresponding Matrimid matter
Measure preparation liquid needed for the mixed substrate membrane containing nano-grade molecular sieve that percentage composition is 95 ~ 70 wt%；The ZIF-7 nano-particle of respective quality is dispersed in three
In chloromethanes, within ultrasonic 30 minutes, ZIF-7 granule is made to be uniformly dispersed；It is dividedly in some parts the Matrimid of respective quality the most wherein,
Stir 48 hours to obtain uniform preparation liquid；Ultrasonic and stir；Stand and prepare knifing；
D. masking
Plate glass and blade applicator are asked wash clean, preparation liquid is uniformly poured on plate glass, use blade applicator at flat board glass
Carry out knifing on glass, taken off after film is dry at once, put in baking oven and anneal 16 hours at 180 DEG C；Final prepared mixed base
Plasma membrane.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106390768A (en) * | 2016-11-14 | 2017-02-15 | 中国工程物理研究院化工材料研究所 | Zeolite imidazate framework/polyamide composite membrane and preparation method thereof |
| CN108159897A (en) * | 2018-01-02 | 2018-06-15 | 天津工业大学 | A kind of PVDF/ZIF-7 hydrophobic membranes and preparation method with dual microtexture |
| CN108452850A (en) * | 2018-03-28 | 2018-08-28 | 江苏师范大学 | A kind of in-situ synthetic method of ZnO/Au heterojunction photocatalysts and the preparation method of ZIF-7 |
| CN108822544A (en) * | 2018-07-09 | 2018-11-16 | 黑龙江科技大学 | A kind of preparation method of polyimides/metal organic framework laminated film |
| CN108939928A (en) * | 2018-06-29 | 2018-12-07 | 中国石油大学(华东) | A kind of preparation method with the nanocrystalline mixed substrate membrane containing nano-grade molecular sieve for filler of sodalite |
| CN109395779A (en) * | 2018-09-21 | 2019-03-01 | 江苏大学 | A kind of preparation method and purposes of the multifunctional solid catalyst based on emulsion template method |
| CN109731437A (en) * | 2019-02-23 | 2019-05-10 | 华南理工大学 | The application of embrane method capture carbon dioxide in a kind of flue gas |
| CN110372872A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院福建物质结构研究所 | The magnanimity of hybrid zeolite imidazoles frame material prepares and morphological control method |
| CN111617645A (en) * | 2020-05-20 | 2020-09-04 | 大连理工大学 | Preparation method of low-resistance high-selectivity mixed matrix membrane based on hollow MOFs (metal-organic frameworks) material |
| CN111841344A (en) * | 2020-07-21 | 2020-10-30 | 浙江大学 | Preparation method of copper-nickel zeolite imidazole ester loaded polyimide gel mixed matrix membrane |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106390768B (en) * | 2016-11-14 | 2019-01-11 | 中国工程物理研究院化工材料研究所 | A kind of zeolite imidazole ester skeleton/polyamide composite film and preparation method thereof |
| CN106390768A (en) * | 2016-11-14 | 2017-02-15 | 中国工程物理研究院化工材料研究所 | Zeolite imidazate framework/polyamide composite membrane and preparation method thereof |
| CN108159897A (en) * | 2018-01-02 | 2018-06-15 | 天津工业大学 | A kind of PVDF/ZIF-7 hydrophobic membranes and preparation method with dual microtexture |
| CN108452850A (en) * | 2018-03-28 | 2018-08-28 | 江苏师范大学 | A kind of in-situ synthetic method of ZnO/Au heterojunction photocatalysts and the preparation method of ZIF-7 |
| CN110372872A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院福建物质结构研究所 | The magnanimity of hybrid zeolite imidazoles frame material prepares and morphological control method |
| CN108939928A (en) * | 2018-06-29 | 2018-12-07 | 中国石油大学(华东) | A kind of preparation method with the nanocrystalline mixed substrate membrane containing nano-grade molecular sieve for filler of sodalite |
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