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Preparation method of high-flux self-supporting MOF glass gas separation membrane for difficult-to-separate system

A gas separation membrane, self-supporting technology, applied in the field of membrane separation, which can solve the problems of low output and high energy consumption

Active Publication Date: 2021-09-07
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the deficiencies of the existing methods, use the ball milling method to overcome the defects of low yield and high energy consumption of the previous hydrothermal method, and prepare the ZIF-62MOF material with small particle size, which provides a new method for industrial preparation; The self-supporting vitrified MOF membrane is prepared in the form of a sheet. The MOF glass membrane without a support body gets rid of the limitation of the flux by the support body, and greatly improves the flux of the membrane. It is suitable for industrial production of CH 4 / N 2 Separation membrane has practical value

Method used

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  • Preparation method of high-flux self-supporting MOF glass gas separation membrane for difficult-to-separate system
  • Preparation method of high-flux self-supporting MOF glass gas separation membrane for difficult-to-separate system
  • Preparation method of high-flux self-supporting MOF glass gas separation membrane for difficult-to-separate system

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Embodiment 1

[0031] A method for preparing a self-supporting MOF glass gas separation membrane with high selectivity and high flux for difficult separation systems, characterized in that it comprises the following steps:

[0032] (1) mix the mixed metal sources and the ligands in different molar ratios uniformly according to a certain molar ratio, use a planetary ball mill to carry out ball milling, carry out suction filtration to the obtained product, wash with methanol, and obtain ZIF-62 particles;

[0033] (2) Calcining the powder obtained in step (1) by using a tube furnace to obtain vitrified ZIF-62.

[0034] (3) The traditional hydrothermal method was used to prepare ZIF-62 powder for comparison with the ball milling method.

[0035] Table 1 shows that the characteristic description that obtains product when metal salt is different mol ratio, can find out that ZIF-62 without impurity can be obtained when the mol ratio of zinc hydroxide and zinc acetate is 70:30, and this is because z...

Embodiment 2

[0044] A method for preparing a self-supporting MOF glass gas separation membrane with high selectivity and high flux for difficult separation systems, characterized in that it comprises the following steps:

[0045](1) get 300 mg of ZIF-62 powder and adopt a mechanical tablet press to prepare discs with a certain diameter and thickness;

[0046] (2) Calcining the disc obtained in step (1) by using a tube furnace to obtain a self-supporting ZIF-62 glass film.

[0047] figure 2 It shows that the membrane surface of the self-supporting vitrified MOF membrane is very dense without defects (A); the cross-section of the membrane is also very dense (B); the thickness of the membrane cross-section is uniform (C). The light transmittance of the glass film is good, in line with the optical properties of glass (D).

Embodiment 3

[0049] A method for preparing a self-supporting MOF glass gas separation membrane with high selectivity and high flux for difficult separation systems, characterized in that it comprises the following steps:

[0050] (1) get the ZIF-62 powder of 400 milligrams and adopt mechanical tabletting machine, be prepared into the disc of certain diameter, thickness;

[0051] (2) Calcining the disc obtained in step (1) by using a tube furnace to obtain a self-supporting ZIF-62 glass film.

[0052] image 3 It shows that the membrane surface of the self-supporting vitrified MOF membrane is very dense without defects (A); the cross-section of the membrane is also very dense (B); the thickness of the membrane cross-section is uniform (C). The light transmittance of the glass film is good, in line with the optical properties of glass (D).

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Abstract

The invention discloses a preparation method of a high-selectivity high-flux self-supporting MOF glass gas separation membrane for a difficult-to-separate system. The preparation process comprises the following steps that firstly, ZIF-62 particles are prepared by adopting a green and environment-friendly ball milling method with high yield and high reaction rate; ZIF-62 powder with the high-temperature melting characteristic is pressed into a wafer with a certain thickness through a mechanical tabletting method, then the wafer is heated in an inert gas atmosphere, the heating temperature needs to guarantee that particles can be melted, and therefore defects and grain boundaries in the wafer are eliminated. According to the preparation method, the MOF material with a melting characteristic is prepared by adopting an environment-friendly ball milling method, and the MOF glass gas separation membrane with a self-supporting characteristic, high separation selectivity and high flux is obtained by combining a tabletting method and a heat treatment method, so that a scheme is provided for separation of difficult-to-separate gas.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, and specifically relates to a method for preparing a self-supporting MOF glass gas separation membrane with high selectivity and high flux for difficult-to-separate systems. Background technique [0002] Membrane separation technology has the advantages of high efficiency, greenness, energy saving, and easy processing, and is considered to be a potential gas separation technology. Microporous inorganic materials with molecular sieve properties, represented by zeolites, have developed as a promising candidate for fabricating high-performance membranes. Over the past decade, metal-organic frameworks (MOFs) have become a hot research topic for membrane materials due to their unique structural and chemical versatility compared with zeolites. However, similar to zeolite membranes, the polycrystalline nature of MOF membranes poses the most demanding challenges for their fabrication and uti...

Claims

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Application Information

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IPC IPC(8): B01D71/06B01D67/00B01D53/22
CPCB01D71/06B01D67/0079B01D53/228
Inventor 仲崇立乔志华杨紫博孙玉绣黄宏亮郭翔宇
Owner TIANJIN POLYTECHNIC UNIV
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