CN110917822A - High-flux high-selectivity thin-layer composite membrane for hydrogen separation and preparation method thereof - Google Patents
High-flux high-selectivity thin-layer composite membrane for hydrogen separation and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-flux high-selectivity thin-layer composite membrane for hydrogen separation and a preparation method thereof, and the preparation method comprises the following steps: adding benzimidazole and zinc nitrate hexahydrate into an organic solvent, standing, centrifuging to obtain ZIF-7 crystal particles, and obtaining layered Zn in boiling water2(bim)4(ii) a Evaporating, ball-milling, dispersing in alcohol, and ultrasonic stripping to obtain two-dimensional Zn2(bim)4The nano sheet is deposited on the upper surface of the ultrafiltration membrane to obtain a substrate; soaking the substrate in an amine or phenol monomer solution, taking out, and removing liquid on the surface of the substrate; and then soaking the substrate upper surface in a n-hexane solution of trimesoyl chloride for interfacial polymerization to obtain the nano-composite material. The high-flux high-selectivity thin-layer composite membrane for hydrogen separation solves the problem of low flux of the traditional thin-layer composite gas separation membrane, and has high H2Flux and high H2/CO2,N2,CH4The selectivity and the method are simple, convenient and mild, and are suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to a high-flux high-selectivity thin-layer composite membrane for hydrogen separation, and a preparation method and application thereof.
Background
The commercial gas separation membrane mainly comprises an ultrathin selective functional layer, an intermediate layer and a porous supporting layer. The low gas flux of the polymeric intermediate layer makes most gas separation membranes difficult to meet for large-scale industrial applications at present. The MOFs (metal organic frameworks) material has the advantages of good size sieving performance, thermal and chemical stability, structural diversity, adjustable pore channels and the like, and becomes a new research hotspot in the field of gas separation in recent years. The two-dimensional MOFs nano-sheet material is an ideal material for gas separation due to the super-large specific surface area and the ultra-thin thickness. Therefore, the thin-layer composite gas separation membrane taking the MOFs material, particularly the two-dimensional MOFs nano-sheet material, as the middle layer is developed, the gas mass transfer resistance of the membrane can be effectively reduced, and the high-performance gas separation membrane is obtained.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-flux high-selectivity thin-layer composite membrane for hydrogen separation.
A second object of the present invention is to provide a method for preparing a high-flux high-selectivity thin-layer composite membrane for hydrogen separation.
A third object of the present invention is to provide the use of a high flux high selectivity thin composite membrane for hydrogen separation.
The technical scheme of the invention is summarized as follows:
a preparation method of a high-flux high-selectivity thin-layer composite membrane for hydrogen separation comprises the following steps:
a. adding 15-45g of benzimidazole and 3-9g of zinc nitrate hexahydrate into 200mL of organic solvent according to the proportion, standing, and centrifuging to obtain ZIF-7 crystal particles; 0.5-1.5g of the ZIF-7 crystal particles are subjected to crystal form conversion for 20-28h in 100mL of boiling waterObtaining layered Zn2(bim)4(ii) a Evaporating to remove 0.5-1.5g of said layered Zn2(bim)4Ball-milling, dispersing into 100mL of alcohol, and ultrasonically stripping for 20-24h to obtain two-dimensional Zn2(bim)4Nanosheets;
b. 0.5-1.5g of said two-dimensional Zn2(bim)4Depositing the nanosheets on the upper surface of the ultrafiltration membrane to obtain a substrate;
c. soaking the substrate in an alkaline aqueous solution of 18-22mmol/L amine or phenol monomer for 3-15 min; taking out, and removing the liquid on the surface of the substrate after soaking; and then soaking the upper surface of the soaked substrate in 0.5-20mmol/L of trimesoyl chloride n-hexane solution for interfacial polymerization to obtain the high-flux high-selectivity thin-layer composite membrane for hydrogen separation.
The organic solvent is at least one of methanol, ethanol, N, N-dimethylformamide, N, N-dimethylacetamide and N-methylpyrrolidone.
The alcohol is at least one of methanol, ethanol, n-propanol and n-octanol.
Two-dimensional Zn2(bim)4The method for depositing the nanosheets on the upper surface of the ultrafiltration membrane is vacuum filtration or electrostatic spraying.
The ultrafiltration membrane is at least one of polysulfone ultrafiltration membrane, polyethersulfone ultrafiltration membrane, polyetherimide ultrafiltration membrane, polyimide ultrafiltration membrane, cellulose acetate ultrafiltration membrane or hydrolyzed polyacrylonitrile ultrafiltration membrane.
The amine is p-phenylenediamine, o-phenylenediamine or m-phenylenediamine.
The phenolic monomer is 5,5,6, 6-tetrahydroxy-3, 3,3,3 tetramethyl spiral bis indane.
The alkali is sodium hydroxide or potassium hydroxide.
The thin-layer composite membrane with high flux and high selectivity for hydrogen separation prepared by the method.
The application of the high-flux high-selectivity thin-layer composite membrane for hydrogen separation in the gas separation process is disclosed.
The high-flux high-selectivity thin-layer composite membrane for hydrogen separation solves the problem of flux of the traditional thin-layer composite gas separation membraneLow problem, it has high H2Flux and high H2/CO2,N2,CH4The selectivity and the method are simple, convenient and mild, and are suitable for industrial production.
Drawings
FIG. 1 is an SEM image of the surface of the substrate prepared in step b of example 1.
Fig. 2 is a surface SEM image of a high-flux high-selectivity thin-layer composite membrane for hydrogen separation prepared in example 1.
FIG. 3 is a Robeson upper bound graph of gas separation performance of a high flux high selectivity thin film composite membrane for hydrogen separation prepared in example 1.
Detailed Description
The present invention will be further described with reference to the following specific examples.
After reading the teaching of the present invention, the skilled in the art can make various changes or modifications to the invention, and these equivalents also fall within the scope of the claims of the present application.
Ultrafiltration membranes to which the examples relate: polysulfone ultrafiltration membranes, polyethersulfone ultrafiltration membranes, polyetherimide ultrafiltration membranes, polyimide ultrafiltration membranes, cellulose acetate ultrafiltration membranes are all commercial products.
The hydrolyzed polyacrylonitrile ultrafiltration membrane is obtained by sequentially soaking a commercial polysulfone ultrafiltration membrane in 2mol/L sodium hydroxide alkaline aqueous solution and 2mol/L acetic acid acidic aqueous solution for 2 hours respectively and carrying out pretreatment.
Example 1
A preparation method of a high-flux high-selectivity thin-layer composite membrane for hydrogen separation comprises the following steps:
a. adding 30g of benzimidazole and 6g of zinc nitrate hexahydrate into 200mL of N-methylpyrrolidone, standing, and centrifuging to obtain ZIF-7 crystal particles; boiling 1g of ZIF-7 crystal particles in 100mL of boiling water for 24h, and converting crystal form to obtain layered Zn2(bim)4(ii) a Evaporating to remove 1g of layered Zn2(bim)4Ball-milling, dispersing into 100mL of methanol, and ultrasonically stripping for 24h under the condition of ultrasonic power of 40K to obtain two-dimensional Zn2(bim)4Nanosheets;
b. 1g of two-dimensional Zn2(bim)4Dispersing the nano-sheets in 100mL of methanol, and carrying out vacuum filtration on the two-dimensional Zn2(bim)4Depositing the nanosheets on the surface of the hydrolyzed polyacrylonitrile ultrafiltration membrane to obtain a substrate (figure 1);
c. soaking the substrate in 20 mmol/L5, 5,6, 6-tetrahydroxy-3, 3,3,3 tetramethyl helix bis indane in sodium hydroxide water solution (pH 12) for 5 min; taking out, and removing the liquid on the surface of the substrate after soaking; and then soaking the upper surface of the soaked substrate in a 20mmol/L n-hexane solution of trimesoyl chloride for 5min for interfacial polymerization to obtain the high-flux high-selectivity thin-layer composite membrane for hydrogen separation (figure 2).
Gas separation performance characterization of high-flux high-selectivity thin-layer composite membrane for hydrogen separation
Single gas (H)2，CO2，N2，CH4) Permeation was tested by a constant feed pressure instrument at room temperature. The gas separation unit was a Datong gas separation unit from Tianjin, measuring the volume of permeated gas and the time to permeate the volume by a soap film flow meter (10mL) and a stopwatch. The permeation flux of a single gas i can be calculated by equation (1):
in the formula Ji(mol·m-2·Pa-1·s-1) For gas permeability, A (m)2) For testing the membrane area,. DELTA.pi(Pa) is the transmembrane pressure difference, Vi(mol) is the product of the permeated gas, ti(s) is a transmission time. Volume and time measurements for each gas were taken at steady state and each gas was tested at least 3 times.
The ideal selectivity for the two gases (i and j) is calculated from equation (2):
forHigh flux high selectivity thin film composite membranes for hydrogen separation exhibit H2The permeation flux is 8.2-10-7molm-2s-1pa-1，H2/CO2,H2/N2,H2/CH4The pure gas selectivity is 12.1, 12.4 and 12.3 respectively. The membrane exhibited a separation permeability to hydrogen gas that exceeded that of a Robeson upper bound (fig. 3).
Example 2
A preparation method of a high-flux high-selectivity thin-layer composite membrane for hydrogen separation comprises the following steps:
a. adding 15g of benzimidazole and 3g of zinc nitrate hexahydrate into 200mL of organic solution (mixed solution of N, N-dimethylformamide and N, N-dimethylacetamide in a volume ratio of 1: 1), standing, and centrifuging to obtain ZIF-7 crystal particles; 0.5g of ZIF-7 crystal particles are subjected to crystal form conversion for 20h in 100mL of boiling water to obtain layered Zn2(bim)4(ii) a Evaporating to remove 0.5g of said layered Zn2(bim)4Ball-milling, dispersing into 100mL alcohol (mixed alcohol of ethanol and n-propanol with the volume ratio of 1: 1), and ultrasonically stripping for 20h under the condition of the ultrasonic power of 40K to obtain two-dimensional Zn2(bim)4Nanosheets;
b. 0.5g of two-dimensional Zn2(bim)4Dispersing the nano-sheets in 100mL of methanol, and carrying out vacuum filtration on the two-dimensional Zn2(bim)4Depositing a nanosheet on the upper surface of the polysulfone ultrafiltration membrane to obtain a substrate;
c. soaking the substrate in an alkaline aqueous solution of 18mmol/L p-phenylenediamine (the alkaline aqueous solution is an aqueous sodium hydroxide solution with the pH value of 12) for 3 min; taking out, and removing the liquid on the surface of the substrate after soaking; and then soaking the upper surface of the soaked substrate in a 0.5mmol/L n-hexane solution of trimesoyl chloride for interfacial polymerization to obtain the high-flux high-selectivity thin-layer composite membrane for hydrogen separation.
Gas separation performance characterization of high-flux high-selectivity thin-layer composite membrane for hydrogen separation
High flux high selectivity thin layer composite membranes for hydrogen separation exhibit H2The permeation flux is 9.8-10-7molm-2s-1pa-1，H2/CO2,H2/N2,H2/CH4The pure gas selectivity is 8.1, 8.6 and 8.2 respectively.
Example 3
A preparation method of a high-flux high-selectivity thin-layer composite membrane for hydrogen separation comprises the following steps:
a. adding 45g of benzimidazole and 9g of zinc nitrate hexahydrate into 200mL of organic solvent (a mixed solution of methanol and ethanol with the volume ratio of 1: 1), standing, and centrifuging to obtain ZIF-7 crystal particles; carrying out crystal form conversion on 1.5g of ZIF-7 crystal particles in 100mL of boiling water for 28h to obtain layered Zn2(bim)4(ii) a Evaporating to remove 1.5g of said layered Zn2(bim)4Ball-milling, dispersing into 100mL of n-octanol, and ultrasonically stripping for 24h under the condition of ultrasonic power of 40K to obtain two-dimensional Zn2(bim)4Nanosheets;
b. 1.5g of the two-dimensional Zn2(bim)4Electrostatically spraying the nanosheets on the upper surface of the polyethersulfone ultrafiltration membrane to obtain a substrate;
c. soaking the substrate in 22mmol/L alkaline aqueous solution of o-phenylenediamine (or metaphenylene diamine) with pH of 12 potassium hydroxide for 15 min; taking out, and removing the liquid on the surface of the substrate after soaking; and then soaking the upper surface of the soaked substrate in 20mmol/L n-hexane solution of trimesoyl chloride for interfacial polymerization to obtain the high-flux high-selectivity thin-layer composite membrane for hydrogen separation.
Gas separation performance characterization of high-flux high-selectivity thin-layer composite membrane for hydrogen separation
High flux high selectivity thin layer composite membranes for hydrogen separation exhibit H2The permeation flux is 6.2-10-7molm-2s-1pa-1，H2/CO2,H2/N2,H2/CH4The pure gas selectivity is 10.1, 10.4 and 10.2 respectively.
The polyether imide ultrafiltration membrane is used for replacing the polyether sulfone ultrafiltration membrane in the embodiment, and other properties are similar to the gas separation performance characterization of the high-flux high-selectivity thin-layer composite membrane for hydrogen separation prepared in the embodiment:
high flux high selectivity thin layer composite membranes for hydrogen separation exhibit H2The permeation flux is 5.7-10-7molm-2s-1pa-1，H2/CO2,H2/N2,H2/CH4The pure gas selectivity is 9.5, 9.9 and 9.2 respectively.
The polyimide ultrafiltration membrane is used for replacing the polyethersulfone ultrafiltration membrane in the embodiment, and other properties are similar to the gas separation performance characterization of the high-flux high-selectivity thin-layer composite membrane for hydrogen separation prepared in the embodiment:
high flux high selectivity thin layer composite membranes for hydrogen separation exhibit H2The permeation flux is 3.2-10-7molm-2s-1pa-1，H2/CO2,H2/N2,H2/CH4The pure gas selectivity is 11.1, 11.4 and 11.2 respectively.
The gas separation performance characterization of the high-flux high-selectivity thin-layer composite membrane for hydrogen separation prepared by using the cellulose acetate ultrafiltration membrane instead of the polyethersulfone ultrafiltration membrane in the embodiment is otherwise the same as that in the embodiment:
high flux high selectivity thin layer composite membranes for hydrogen separation exhibit H2The permeation flux is 7.8-10-7molm-2s-1pa-1，H2/CO2,H2/N2,H2/CH4The pure gas selectivity is 9.7, 10.2 and 9.9 respectively.
Claims (10)
1. A preparation method of a high-flux high-selectivity thin-layer composite membrane for hydrogen separation is characterized by comprising the following steps:
a. adding 15-45g of benzimidazole and 3-9g of zinc nitrate hexahydrate into 200mL of organic solvent according to the proportion, standing, and centrifuging to obtain ZIF-7 crystal particles; 0.5-1.5g of ZIF-7 crystal particles are subjected to crystal form conversion for 20-28h in 100mL of boiling water to obtain layered Zn2(bim)4(ii) a Evaporating to remove 0.5-1.5g of said layered Zn2(bim)4Ball-milling, dispersing into 100mL of alcohol, and ultrasonically stripping for 20-24h to obtain two-dimensional Zn2(bim)4Nanosheets;
b. 0.5-1.5g of said two-dimensional Zn2(bim)4Depositing the nanosheets on the upper surface of the ultrafiltration membrane to obtain a substrate;
c. soaking the substrate in an alkaline aqueous solution of 18-22mmol/L amine or phenol monomer for 3-15 min; taking out, and removing the liquid on the surface of the substrate after soaking; and then soaking the upper surface of the soaked substrate in 0.5-20mmol/L of trimesoyl chloride n-hexane solution for interfacial polymerization to obtain the high-flux high-selectivity thin-layer composite membrane for hydrogen separation.
2. The method as set forth in claim 1, wherein the organic solvent is at least one of methanol, ethanol, N, N-dimethylformamide, N, N-dimethylacetamide and N-methylpyrrolidone.
3. The method according to claim 1, wherein the alcohol is at least one of methanol, ethanol, n-propanol and n-octanol.
4. The method as set forth in claim 1, wherein Zn is expressed in two dimensions2(bim)4The method for depositing the nanosheets on the upper surface of the ultrafiltration membrane is vacuum filtration or electrostatic spraying.
5. The method of claim 1, wherein the ultrafiltration membrane is at least one of a polysulfone ultrafiltration membrane, a polyethersulfone ultrafiltration membrane, a polyetherimide ultrafiltration membrane, a polyimide ultrafiltration membrane, a cellulose acetate ultrafiltration membrane, or a hydrolyzed polyacrylonitrile ultrafiltration membrane.
6. The method as set forth in claim 1, wherein the amine is p-phenylenediamine, o-phenylenediamine or m-phenylenediamine.
7. The method as set forth in claim 1, wherein said phenolic monomer is 5,5,6, 6-tetrahydroxy-3, 3,3,3 tetramethylspirobiindane.
8. The method as set forth in claim 1, wherein the alkali is sodium hydroxide or potassium hydroxide.
9. A high flux high selectivity thin layer composite membrane for hydrogen separation prepared by the method of any one of claims 1 to 8.
10. Use of a high flux high selectivity thin layer composite membrane for hydrogen separation according to claim 9 in a gas separation process.
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| CN113522040A (en) * | 2021-07-30 | 2021-10-22 | 天津大学 | Method for preparing high-performance carbon dioxide separation composite membrane containing twisted structure through interfacial polymerization |
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| CN116574264A (en) * | 2023-04-14 | 2023-08-11 | 华南理工大学 | Ultra-thin two-dimensional MOF nanosheet combining ball milling and cell crushing and ultrasonic stripping as well as preparation method and application thereof |
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