CN112705056A - Method for rapidly preparing two-dimensional zeolite molecular sieve membrane by electrophoretic deposition and two-dimensional zeolite molecular sieve membrane prepared by method - Google Patents
Method for rapidly preparing two-dimensional zeolite molecular sieve membrane by electrophoretic deposition and two-dimensional zeolite molecular sieve membrane prepared by method Download PDFInfo
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- CN112705056A CN112705056A CN202011547365.8A CN202011547365A CN112705056A CN 112705056 A CN112705056 A CN 112705056A CN 202011547365 A CN202011547365 A CN 202011547365A CN 112705056 A CN112705056 A CN 112705056A
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- molecular sieve
- electrophoretic deposition
- sieve membrane
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0069—Inorganic membrane manufacture by deposition from the liquid phase, e.g. electrochemical deposition
Abstract
The invention belongs to the technical field of preparation of nano separation membranes, and discloses a method for quickly preparing a two-dimensional zeolite molecular sieve membrane by electrophoretic deposition and the prepared two-dimensional zeolite molecular sieve membrane. The method specifically comprises the following steps: (1) dispersing zeolite nanosheet powder in a solvent, and performing ultrasonic assistance to obtain a zeolite nanosheet solution; (2) carrying out electrophoretic deposition on the zeolite nanosheet solution, and drying to obtain a two-dimensional zeolite molecular sieve membrane; the electrophoretic deposition condition is 1 mV-1000V, and the electrophoretic deposition time is 1 s-100 h. The method is simple and efficient, saves time and has low cost.
Description
Technical Field
The invention belongs to the technical field of preparation of nano separation membranes, and particularly relates to a method for quickly preparing a two-dimensional zeolite molecular sieve membrane by electrophoretic deposition and the prepared two-dimensional zeolite molecular sieve membrane.
Background
With the increasing pressure of energy crisis and environment, the membrane separation technology has the advantages of high separation efficiency, no phase change, energy saving, easy control and continuous operation in highly integrated equipment, is widely applied to the fields of chemical industry, food, medicine, biology, environment and the like, and becomes one of the very important means in the current separation process. At present, the membrane separation technology will improve and perfect the existing membrane process on one hand, and continuously explore and develop new processes and materials on the other hand, and continuously expand the original application field.
Polymer membranes, which have always led to the membrane market, cannot simultaneously have high permeability and high selectivity, and therefore one of the main goals in the development of new membrane materials is to go beyond the so-called "Robeson's upper bound". Pore structures with well-defined molecular dimensions can achieve the goal of high selectivity (efficiency) through a precise molecular sieve mechanism, while a key issue in increasing membrane permeability is reducing membrane thickness to nanometer and even sub-nanometer dimensions. From this perspective, two-dimensional molecular sieve materials or molecular sieve nanoplates have unique advantages.
The zeolite molecular sieve has the advantages of high porosity, clear aperture, good chemical stability and thermal stability and the like, and the two-dimensional molecular sieve membrane with the short mass transfer channel is constructed by stacking the two-dimensional zeolite nanosheets, so that the mass transfer efficiency and the permeation flux can be improved. At present, the synthesis methods of two-dimensional zeolite molecular sieves are mainly divided into three methods, namely solvothermal method, surfactant template synthesis and ADOR (assembly-disassembly-organization-recombination). The electrophoretic deposition method has the advantages of high deposition rate, controllable thickness, good uniformity, easy obtaining of a film with larger area and the like in the aspect of preparing the film, and is a technology with high efficiency and wide application prospect. The solvothermal method has reversibility and limited production efficiency; the ADOR method has stronger selectivity, but the energy consumption of the method for preparing IPC-9 and IPC-10 by the Michal subject group through high-temperature calcination for a certain time is larger.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a method for rapidly preparing a two-dimensional zeolite molecular sieve membrane by electrophoretic deposition and the two-dimensional zeolite molecular sieve membrane prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a method for rapidly preparing a two-dimensional zeolite molecular sieve membrane by an electrophoretic deposition method comprises the following steps:
(1) dispersing zeolite nanosheet powder in a solvent, and performing ultrasonic assistance to obtain a zeolite nanosheet solution;
(2) carrying out electrophoretic deposition on the zeolite nanosheet solution in the step (1), and drying to obtain a two-dimensional zeolite molecular sieve membrane; the electrophoretic deposition condition is 1 mV-1000V, and the electrophoretic deposition time is 1 s-100 h.
Preferably, the zeolite nano-sheet powder in the step (1) is one of MWW, MFI, IPC-9, IPC-10, ZSM-5, FER, AFO, CDO, HEU and NSI.
Preferably, the solvent in step (1) is one or more of water, ethanol, toluene, choline hydroxide, choline chloride, hexadecyl trimethyl ammonium hydroxide, N-dimethylformamide and the like.
Preferably, the amount of the zeolite nanosheet powder and the solvent used in step (1) is 1g of zeolite nanosheet powder: (1-9000) mL of a solvent; the zeolite nanosheet powder is a dry product.
Preferably, the ultrasonic time in the step (1) is 5 s-100 h.
Preferably, the concentration of the zeolite nanosheet solution in step (1) is 0.1-1000 mg/mL.
Preferably, the working electrode in the electrophoretic deposition in the step (2) is a non-porous substrate or a porous substrate.
Preferably, the drying in step (2) is vacuum drying.
The two-dimensional zeolite molecular sieve membrane prepared by the method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention can save a large amount of time to obtain the membrane with the same thickness compared with other methods when preparing the zeolite molecular sieve membrane, and has high efficiency.
(2) The two-dimensional zeolite molecular sieve membrane used in the invention has the advantages of simple preparation method and low cost, and has great potential in the aspect of industrial large-scale production.
Detailed Description
The present invention is described in further detail with reference to examples, but the embodiments and the scope of the present invention are not limited thereto.
Example 1
(1) Dispersing 10g of dried MWW zeolite nanosheet powder in 100ml of water, and performing ultrasonic assistance for 1h to obtain a zeolite nanosheet solution;
(2) and (2) taking a non-porous substrate as a working electrode, setting a voltage of 50V, carrying out electrophoretic deposition on the zeolite nanosheet solution in the step (1) for 5 hours, and drying in vacuum to obtain the two-dimensional zeolite molecular sieve membrane.
Example 2
(1) Dispersing 10g of dried MFI zeolite nanosheet powder in 500ml of ethanol, and performing ultrasonic assistance for 0.5h to obtain a zeolite nanosheet solution;
(2) and (2) taking a non-porous substrate as a working electrode, setting a voltage of 5V, carrying out electrophoretic deposition on the zeolite nanosheet solution in the step (1) for 20h, and drying in vacuum to obtain the two-dimensional zeolite molecular sieve membrane.
Example 3
(1) Dispersing 10g of dried IPC-9 zeolite nanosheet powder in 50ml of toluene, and carrying out ultrasonic assistance for 5 hours to obtain a zeolite nanosheet solution;
(2) and (2) setting a voltage of 100V by taking a porous substrate as a working electrode, carrying out electrophoretic deposition on the zeolite nanosheet solution in the step (1) for 0.5h, and drying in vacuum to obtain the two-dimensional zeolite molecular sieve membrane.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A method for rapidly preparing a two-dimensional zeolite molecular sieve membrane by electrophoretic deposition is characterized by comprising the following steps:
(1) dispersing zeolite nanosheet powder in a solvent, and performing ultrasonic assistance to obtain a zeolite nanosheet solution;
(2) carrying out electrophoretic deposition on the zeolite nanosheet solution in the step (1), and drying to obtain a two-dimensional zeolite molecular sieve membrane; the electrophoretic deposition condition is 1 mV-1000V, and the electrophoretic deposition time is 1 s-100 h.
2. The method for rapidly preparing the two-dimensional zeolite molecular sieve membrane by electrophoretic deposition according to claim 1, wherein the zeolite nanosheet powder in step (1) is one of MWW, MFI, IPC-9, IPC-10, ZSM-5, FER, AFO, CDO, HEU, and NSI.
3. The method for rapidly preparing a two-dimensional zeolite molecular sieve membrane by electrophoretic deposition according to claim 1, wherein the solvent in step (1) is one or more of water, ethanol, toluene, choline hydroxide, choline chloride, hexadecyl trimethyl ammonium hydroxide and N, N-dimethylformamide.
4. The method for rapidly preparing the two-dimensional zeolite molecular sieve membrane by electrophoretic deposition according to claim 1, wherein the dosage ratio of the zeolite nanosheet powder to the solvent in step (1) is 1g of zeolite nanosheet powder: (1-9000) mL of a solvent; the zeolite nanosheet powder is a dry product.
5. The method for rapidly preparing the two-dimensional zeolite molecular sieve membrane by electrophoretic deposition according to claim 1, wherein the time of the ultrasonic treatment in the step (1) is 5 s-100 h; the concentration of the zeolite nanosheet solution in the step (1) is 0.1-1000 mg/mL.
6. The method for rapidly preparing the two-dimensional zeolite molecular sieve membrane by electrophoretic deposition according to claim 1, wherein the working electrode of electrophoretic deposition in step (2) is a non-porous substrate or a porous substrate; the drying in the step (2) is vacuum drying.
7. A two-dimensional zeolitic molecular sieve membrane prepared by the method of any of claims 1-6.
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| CN202011547365.8A CN112705056B (en) | 2020-12-23 | 2020-12-23 | Method for rapidly preparing two-dimensional zeolite molecular sieve membrane by electrophoretic deposition and two-dimensional zeolite molecular sieve membrane prepared by method |
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| CN114522543A (en) * | 2022-01-19 | 2022-05-24 | 华南理工大学 | Ultrathin two-dimensional Cu-TCPP film and preparation method thereof |
| CN114534509A (en) * | 2022-01-19 | 2022-05-27 | 华南理工大学 | Two-dimensional metal organic framework film and electrophoretic deposition preparation method thereof |
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| EP2138222A1 (en) * | 2008-06-27 | 2009-12-30 | George P. Sakellaropoulos | Method for pore size modification of an inorganic membrane by chemical vapor infiltration |
| CN105350054A (en) * | 2015-11-25 | 2016-02-24 | 哈尔滨工业大学 | Method for modifying nano-carbon material on surface of secondary battery diaphragm through electrophoretic deposition |
| CN106835245A (en) * | 2017-02-24 | 2017-06-13 | 中国科学院上海高等研究院 | A kind of preparation method of the ultra-thin graphene oxide film for molecule screening |
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| EP2138222A1 (en) * | 2008-06-27 | 2009-12-30 | George P. Sakellaropoulos | Method for pore size modification of an inorganic membrane by chemical vapor infiltration |
| CN105350054A (en) * | 2015-11-25 | 2016-02-24 | 哈尔滨工业大学 | Method for modifying nano-carbon material on surface of secondary battery diaphragm through electrophoretic deposition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114522543A (en) * | 2022-01-19 | 2022-05-24 | 华南理工大学 | Ultrathin two-dimensional Cu-TCPP film and preparation method thereof |
| CN114534509A (en) * | 2022-01-19 | 2022-05-27 | 华南理工大学 | Two-dimensional metal organic framework film and electrophoretic deposition preparation method thereof |
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