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A kind of in situ controllable synthesis method of MOF film

A synthesis method and MOF technology, applied in the field of in-situ controllable synthesis of MOF membranes, can solve the problems of material, energy consumption, long and complicated preparation process, difficult limitation and regulation, etc. Effect

Active Publication Date: 2022-01-28
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The fundamental reason is that the in-situ crystallization method is mostly a homogeneous nucleation mechanism, the nucleation process is random and dispersed, and it is difficult to limit and control
As mentioned above, the current solution either starts from the carrier or from the external reaction conditions, which undoubtedly makes the preparation process tedious and complicated, and is accompanied by a large amount of material and energy consumption.

Method used

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  • A kind of in situ controllable synthesis method of MOF film
  • A kind of in situ controllable synthesis method of MOF film
  • A kind of in situ controllable synthesis method of MOF film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Zn 2 (bim) 4 Preparation of molecular sieve membrane

[0034] Metal ion solution preparation: take 0.01116g of zinc nitrate hexahydrate, add 20ml of methanol to dissolve and set aside.

[0035] Organic ligand solution preparation: take 0.02890g of benzimidazole, add 20ml of methanol to dissolve and set aside.

[0036] Carrier: a porous α-alumina disc with a diameter of 18mm and a thickness of 1mm. The carrier has an asymmetric structure. The surface pore size is about 70nm, which is the front side, and the bottom pore size is about 2μm, which is the back side. The carrier is used before use. deionized water and acetone, and then dried before use.

[0037] The carrier impregnation method is negative pressure solution filtration, that is, the carrier is fixed on the device (such as figure 1 The device shown), face up, add the metal ion solution above the carrier, and then filter with suction to make the solution permeate from the carrier.

[0038] Reaction: add the o...

Embodiment 2

[0044] Zn 2 (bim) 4 Preparation of molecular sieve membrane

[0045] Metal ion solution preparation: take 0.01116g of zinc nitrate hexahydrate, add 20ml of methanol to dissolve and set aside.

[0046] Organic ligand solution preparation: take 0.02890g of benzimidazole, add 20ml of methanol to dissolve and set aside.

[0047] Carrier: a porous α-alumina disc with a diameter of 18mm and a thickness of 1mm. The carrier has an asymmetric structure. The surface pore size is about 70nm, which is the front side, and the bottom pore size is about 2μm, which is the back side. The carrier is used before use. deionized water and acetone, and then dried before use.

[0048] According to the same operation as in Example 1, the number of reactions is changed, that is, the membrane after impregnation, reaction, and cleaning is fixed again, and the process of impregnation, reaction, and cleaning is repeated once or twice, and finally the membrane is dried to obtain Zn 2 (bim) 4 Molecular...

Embodiment 3

[0051] Zn 2 (bim) 4 Preparation of molecular sieve membrane

[0052] Preparation of metal ion complex solution: zinc porphyrin / DMF, concentration 0.02mol / L, stir well and set aside.

[0053] Organic ligand solution preparation: benzimidazole / methanol, 0.026mol / L, stir well and set aside.

[0054] Carrier: a porous α-alumina disc with a diameter of 18mm and a thickness of 1mm. The carrier has an asymmetric structure. The surface pore size is about 70nm, which is the front side, and the bottom pore size is about 2μm, which is the back side. The carrier is used before use. deionized water and acetone, and then dried before use.

[0055] The carrier impregnation method is solution pulling impregnation, that is, the carrier is fixed on the pulling machine, and the Zn 2+ - Lifting with porphyrin solution, the lifting can be repeated many times, and drying is carried out after the lifting is completed.

[0056] Reaction: add the organic ligand solution directly on the impregnate...

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Abstract

An in-situ controllable synthesis method of a MOF membrane, in which one side of a porous carrier is placed in a solution metal ion solution A for pre-impregnation treatment, so that the solution A is adsorbed in the pores of the carrier. Fix the impregnated carrier in a self-made stainless steel reaction tank, introduce organic ligand solution B on one side of the pre-impregnated carrier, seal the reaction tank, and start the synthesis reaction at a certain temperature and time. After solvent cleaning and drying, a uniform and dense continuous film is finally obtained, which can be grown repeatedly. The preparation method of the MOF membrane of the present invention is simple and easy, suitable for industrial scale-up, and can be applied to many fields, such as gas separation, liquid separation, sensors, adsorption, functional coating and other fields.

Description

technical field [0001] The invention belongs to the fields of membrane separation, inorganic synthesis, etc., and specifically relates to an in-situ controllable synthesis method of MOF membranes. Background technique [0002] Metal-organic frameworks are a new class of porous crystalline materials with rich composition and adjustable pore structure, which can be widely used in the field of gas and liquid separation, such as for CO 2 Selective adsorption of and related mixtures (such as CO 2 / H 2 , CO 2 / N 2 ), separation of low-carbon hydrocarbons, ketones, and adsorption separation of some biomass platform compounds. [0003] The continuous thin layer formed by MOF grains on the surface of the carrier is called MOF film. Relying on MOF membranes for separation is considered to be one of the most potential high-end separation technologies. The preparation methods of MOF films are mainly prepared by in-situ crystallization method and secondary growth method. Literatur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D67/00B01D69/10B01D71/06C08G83/00
CPCB01D67/0006B01D69/105B01D71/06C08G83/008
Inventor 杨维慎杨昆班宇杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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