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Method for preparing metallic organic frame films

A technology of metal-organic frameworks and metals, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of weak binding force, low carrier nucleation density and difficulty in film formation, etc., and achieve a wide applicability Effect

Inactive Publication Date: 2010-11-24
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is the technical problem that the metal-organic framework has a weak binding force with non-metallic material carriers such as ceramics, which leads to the low nucleation density of the carrier and is not easy to form a film. It provides a continuous and dense MOFs film without cracks. The combined method makes it possible to successfully prepare a continuous, dense, crack-free and defect-free MOFs membrane on the surface of a tubular carrier, which has high industrial application value but is difficult to form a film, and has high-efficiency separation performance for small molecule gases. It is a MOFs material A big step forward in membrane engineering

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1 Cu on the α-alumina tube carrier 3 (BTC) 2 Synthetic Preparation of Membranes

[0019] Carrier pretreatment and modification: Polish the surface of the α-alumina tube carrier with 800# and 1200# sandpaper in sequence until the surface of the carrier is smooth, soak in acid and alkali for 24 hours, and then use ultrasonic vibration to wash away the residue in the hole Alkali, then washed with deionized water until neutral, then dried naturally, and finally dried at a temperature of 423K for later use.

[0020] Soak the pretreated carrier tube in an ethanol solution for a few days and then dry it in an oven, so that the surface of the carrier has -OH groups, and the -OH on the carrier can be combined with Cu 3 (BTC) 2 The organic ligand phase of the complex connects and strengthens Cu 3 (BTC) 2 Film-forming ability on the support.

[0021] Preparation of the seed layer: seal the two ends of the modified carrier tube with polytetrafluoroethylene to prevent ...

Embodiment 2

[0024] Example 2 Zn on the α-alumina tube carrier 4 O(R 1 -BDC) 3 (MOF-5, R 1 =H) Synthetic preparation of membrane

[0025] Carrier modification: soak the pretreated carrier tube in acetic acid solution for a few days and then dry it in an oven, so that the surface of the carrier has -COOH groups, and the -COOH on the carrier can combine with the organic Ligand phase linking enhances the film-forming ability of MOF-5 on the carrier.

[0026] Preparation of the seed layer: seal the two ends of the modified carrier tube with polytetrafluoroethylene to prevent the seed liquid from entering the tube, seal the bottom end of the tubular basement membrane, connect the upper end to the water pump, fix the basement membrane vertically and immerse it in the filled In the glass tube of the prepared MOF-5 seed crystal suspension, turn on the switch of the water pump, adjust the pressure difference between the inside and outside of the basement membrane to 8-10kPa, make the basement m...

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Abstract

The invention belongs to the technical field of novel materials, and relates to a method for preparing metallic organic frame films(MOFs). The method is characterized in that: after a pretreated carrier is modified or not modified and coated or not coated with a crystal seed layer, the low-high temperature crystallization is performed by changing a reaction temperature; by controlling a relative speed between nucleation and crystal growth, a great deal of nuclei are formed on the surface of the carrier at the low-temperature stage, and the nuclei formed at the high-temperature stage are quickly grown; and thus, the metallic organic frame separation film which is dense, continuous, firm, free of cracks and defects and possesses higher separation performance on a micromolecular system is prepared on the carrier. The invention solves the problem that the bonding force between the metallic frame organic matters and the carrier is weak, the problem that the nucleus forming density on the carrier is so low that the continuous dense MOFs film is difficultly formed on the carrier, and provides a method for preparing the metallic organic frame films(MOFs) which are easily operated and controlled, in particular, the metallic organic frame films(MOFs) with the high separation performance prepared on the tube-shaped carrier.

Description

technical field [0001] The invention belongs to the technical field of new materials, and relates to a method for preparing dense, continuous and crack-free metal-organic frameworks (metal-organic frameworks, MOFs) membranes on the surface of tubular or sheet-shaped carriers, and applying the same to the separation of gases. In particular, it relates to the synthesis of metal-organic framework membranes by two-step variable temperature crystallization first at low temperature and then at high temperature and its application to the separation of molecular mixtures. Background technique [0002] The remarkable features of membrane science and technology are energy saving, clean, high efficiency, and strong compatibility. It is suitable for modern industry's needs for energy saving, raw material reuse and elimination of environmental pollution, and has become an important part of the sustainable economic development strategy. Due to its excellent thermal and chemical stability ...

Claims

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Application Information

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IPC IPC(8): B01D69/12B01D71/06
Inventor 杨建华贺广凤王金渠鲁金明张艳殷德宏
Owner DALIAN UNIV OF TECH
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