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Preparation method and application of a ligand-doped metal-organic framework hybrid zif-8 film

A technology of ZIF-8 and ligands, applied in chemical instruments and methods, separation methods, membrane technology, etc., can solve problems such as poor repeatability, reduced gas separation performance, and decreased gas separation selectivity

Active Publication Date: 2022-05-17
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to improve the poor repeatability of the existing ZIF-8 membrane, and the flexibility of the ZIF-8 material skeleton under external stimulation conditions, resulting in a significant decline in gas separation selectivity, and to provide a method for improving ZIF by ligand exchange. The gas separation performance of ZIF-8 membrane, through the introduction of ligands with large steric hindrance during the preparation process, can effectively limit the flipping movement of ligands in the framework, thereby reducing the effective pore size and improving the propylene / propane gas separation performance of ZIF-8 membranes

Method used

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  • Preparation method and application of a ligand-doped metal-organic framework hybrid zif-8 film
  • Preparation method and application of a ligand-doped metal-organic framework hybrid zif-8 film
  • Preparation method and application of a ligand-doped metal-organic framework hybrid zif-8 film

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Experimental program
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Effect test

Embodiment 1

[0081] (1) Carrier pretreatment: Use 600# and 1000# sandpaper to polish the surface of the porous alumina carrier until smooth, then place the carrier in clean water for 10 minutes and ultrasonic frequency is 120KHz, put it in a 300°C muffle after drying Calcined in the furnace for 5 hours, taken out, and used as a carrier for subsequent use;

[0082] (2) Crystal synthesis:

[0083] 0.74 g of zinc nitrate and (22.7-x) g of 2-methylimidazole and x g of 2-aminobenzimidazole were dissolved in 88 g of deionized water at 0.227, 1.135, 2.27, 4.54 and 6.81, respectively, to form a seed solution, 40 ℃ for 4 hours, after centrifugation, washing and drying, 1# hybrid ZIF-8 nanocrystals, 2# hybrid ZIF-8 nanocrystals, 3# hybrid ZIF-8 nanocrystals, and 4# hybrid ZIF-8 nanocrystals were obtained. crystals and 5# hybrid ZIF-8 nanocrystals.

[0084] Wherein in the raw material of 1# hybrid ZIF-8 nanocrystal, the mass ratio of 2-aminobenzimidazole and 2-methylimidazole is 1%,

[0085] Where...

Embodiment 2

[0113] (1) Carrier pretreatment: Use 600# and 1000# sandpaper to polish the surface of the porous alumina carrier until smooth, then place the carrier in clean water for 10 minutes and ultrasonic frequency is 120KHz, put it in a 300°C muffle after drying Calcined in the furnace for 5 hours, taken out, and used as a carrier for subsequent use;

[0114] (2) Crystal synthesis: Dissolve 0.74g of zinc nitrate, 21.565g of 2-methylimidazole and 1.135g of 2-aminobenzimidazole in 88g of deionized water to form a seed crystal solution, react at 50°C for 5h, centrifuge, wash and dry Finally, 6# hybrid ZIF-8 nanocrystals were obtained.

[0115] (3) Polycrystalline film synthesis:

[0116] 6# hybrid ZIF-8 nanocrystals were evenly dispersed in methanol solution to make a 0.1wt% crystal solution, and then the crystal solution was spread on the surface of the carrier by dip coating to form the carrier of 6# pre-coated seed crystals.

[0117] Dissolve 0.07g of zinc nitrate and 2.27g of 2-met...

Embodiment 3

[0121] (1) Carrier pretreatment: Use 600# and 1000# sandpaper to polish the surface of the porous alumina carrier until smooth, then place the carrier in clean water for 10 minutes and ultrasonic frequency is 120KHz, put it in a 300°C muffle after drying Calcined in the furnace for 5 hours, taken out, and used as a carrier for subsequent use;

[0122] (2) Crystal synthesis: 0.74g of zinc nitrate and 22.7g of 2-methylimidazole were dissolved in 88g of deionized water, stirred at 60°C for 5h, centrifuged, washed and dried to obtain 7# ZIF-8 nanocrystals.

[0123] (3) Polycrystalline film synthesis:

[0124] 7# ZIF-8 nanocrystals were uniformly dispersed in DMF solution to make a 0.1wt% crystal solution, and finally the crystal solution was spread on the surface of the carrier by dip coating to form the carrier of 7# pre-coated seed crystals.

[0125] Dissolve 0.07g of zinc nitrate, 2.156g of 2-methylimidazole and 0.113g of 2-aminobenzimidazole in 44g of deionized water, stir fo...

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Abstract

The invention provides a preparation method of a ligand-doped metal-organic framework hybrid ZIF-8 film, which is doped with a first ligand and a second ligand in the ZIF-8 film, the second ligand Introduced in at least one of the seed crystal solution and the secondary growth solution. In this application, the introduction of a ligand with a large steric hindrance in the preparation process can effectively enhance the "rigidity" of the Zn-N bond in the ZIF-8 framework, limit the flipping movement of the ligand, and thus significantly improve the ZIF-8 membrane. gas separation performance. Compared with the traditional ZIF-8 membrane preparation method, the new method adopted in the present invention improves the effective quality of the membrane, and has potential application prospects and extensive application value for industrial propylene / propane separation. The application also discloses that the hybrid ZIF-8 membrane can selectively separate C 3 h 6 / C 3 h 8 Applications in mixed gases. Has a better effect.

Description

technical field [0001] The invention belongs to the technical field of gas separation membranes, and relates to a preparation method and application of a ligand-doped metal-organic framework hybrid ZIF-8 membrane. Background technique [0002] Cryogenic rectification separation of propylene / propane mixed gas is the main means to obtain high-purity propylene in industry. Because propylene and propane have very similar molecular structures and physical and chemical properties, separation is extremely difficult, requiring large investment in equipment and high energy consumption in operation. It is currently one of the most energy-consuming processes in petrochemical industry. Compared with traditional separation technologies, gas separation membrane technology is considered to be a new technology that can potentially replace cryogenic distillation technology to separate propylene / propane mixed gas with low energy consumption due to its advantages of high efficiency, energy sav...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/06B01D67/00B01D53/22
CPCB01D71/06B01D53/228B01D67/0002Y02P20/151
Inventor 潘宜昌宋二悦廉海乾邢卫红
Owner NANJING TECH UNIV
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