Method for preparing silane cross-linked MOFs separation membrane

A silane cross-linking and separation membrane technology, which is applied in separation methods, semipermeable membrane separation, and dispersed particle separation, can solve problems such as easy shedding and defects, and achieve low cost, high temperature resistance, and simple preparation process Effect

Active Publication Date: 2021-04-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to solve the metal-organic framework materials (MOFs) that exist in the prior art as a separation function layer, which is prone to fall off or have defects during use, and provides a new method for preparing silane crosslinked MOFs separation membranes method, first prepare MOFs crystal material, then deposit a layer of MOFs adsorption functional layer on the surface of the substrate by means of filtration deposition, then prepare a siloxane protective layer on the outer surface of the functional layer, and finally prepare an organic separation membrane with a three-layer structure, Therefore, this type of organic gas separation membrane has greater separation coefficient, flux, anti-sticking, anti-pollution and other properties in the application process, and can be better used in the field of organic matter separation

Method used

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  • Method for preparing silane cross-linked MOFs separation membrane
  • Method for preparing silane cross-linked MOFs separation membrane
  • Method for preparing silane cross-linked MOFs separation membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0052] (1) Preparation of the first mixed solution: N, N-dimethylpyrrolidone, terephthalic acid, zirconium tetrachloride are mixed according to the molar ratio of 480:1:1 and fully stirred to obtain the MOFs film preparation required solution;

[0053] (2) Preparation of MOFs material: Put the MOFs preparation solution into the reactor, seal the reactor, add nitrogen protection to discharge water vapor and oxygen. Then put it into a heater at 120° C. under a pressure of 0.1 MPa, and conduct a solvothermal reaction for 48 hours. After the reaction was completed, the reacted solution and crystals were taken out, and the unpolymerized monomer and solvent in the MOFs adsorbent were washed with ethanol for 3 times to obtain a pure MOFs material.

[0054] (3) Formation of MOFs deposition layer:

[0055] (3A) The polyvinylidene fluoride (PVDF) flat ultrafiltration membrane with a pore size of 500nm is made into a plate and frame assembly, and then the surface and internal pollutant...

Embodiment 2

[0063] (1) Preparation of the first mixed solution: N, N-dimethylpyrrolidone, terephthalic acid, zirconium tetrachloride are mixed according to the molar ratio of 100:1:1 and fully stirred to obtain the MOF film preparation required solution;

[0064] (2) Preparation of MOFs material: Put the MOFs preparation solution into the reactor, seal the reactor, add nitrogen protection to discharge water vapor and oxygen. Then put it into a heater at 200° C. under a pressure of 0.1 MPa, and perform a solvothermal reaction for 2 hours. After the reaction is completed, the reacted solution and crystals are taken out, and the unpolymerized monomer and solvent in the MOFs adsorbent are washed with ethanol several times to obtain a pure MOFs material.

[0065] (3) Formation of MOFs deposition layer:

[0066] (3A) The polytetrafluoroethylene tubular microfiltration membrane is made into a module with a pore size of 1000 nm, and then the surface and internal pollutants of the carrier (membr...

Embodiment 3

[0074] (1) Preparation of the first mixed solution: N, N-dimethylpyrrolidone, terephthalic acid, zirconium tetrachloride are mixed according to the molar ratio of 1000:1:1 and fully stirred to obtain the required MOFs film preparation solution;

[0075] (2) Preparation of MOFs material: Put the MOFs preparation solution into the reactor, seal the reactor, add nitrogen protection to discharge water vapor and oxygen. Then put it into a heater at 120° C. under a pressure of 0.2 MPa, and perform a solvothermal reaction for 48 hours. After the reaction is completed, the reacted solution and crystals are taken out, and the unpolymerized monomer and solvent in the MOFs adsorbent are washed with ethanol several times to obtain a pure MOFs material.

[0076] (3) Formation of MOFs deposition layer:

[0077] (3A) The polytetrafluoroethylene tubular microfiltration membrane is made into a module with an average pore size of 500 nm, and then the surface and internal pollutants of the car...

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Abstract

The invention provides a method for preparing a silane cross-linked MOFs separation membrane, which comprises the following steps: (1) preparing a first mixed solution containing N, N-dimethyl pyrrolidone, terephthalic acid and zirconium tetrachloride; (2) heating the first mixed solution, and carrying out a reaction to prepare an MOFs material; (3) depositing the MOFs material prepared in the step (2) in holes of a base membrane and on the surface of the base membrane to form an MOFs deposition layer, so as to obtain a separation membrane with an MOFs deposition layer; (4) coating the surface of the separation membrane prepared in the step (3) with a silane coating solution; and (5) heating the separation membrane obtained in the step (4) to enable the silane coating liquid to be subjected to a cross-linking reaction. The separation membrane with a three-layer structure is prepared, so that the organic gas separation membrane has the properties of larger separation coefficient, flux, adhesion resistance, pollution resistance and the like in the application process, and can be better applied to the field of organic matter separation.

Description

technical field [0001] The invention relates to a method for preparing a silane-crosslinked MOFs separation membrane and the application of the silane-crosslinked MOFs separation membrane prepared by the method in separating organic matter, belonging to the technical field of preparation of organic gas separation membranes. Background technique [0002] There are several definitions of VOCs (Volatile Organic Compounds), and the United States defines it as any organic compound that can participate in atmospheric photochemical reactions. In my country, VOCs refer to organic substances with a saturated vapor pressure greater than 70Pa at normal temperature and a boiling point below 260°C at normal pressure. VOCs contain a variety of organic compounds, usually referring to organic compounds that are easily volatile under normal temperature and pressure, such as benzene, toluene, xylene, acetone, styrene, etc. VOCs mainly come from petrochemical, electronic manufacturing and aut...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B01D67/00B01D69/02B01D69/12B01J20/22B01J20/30B01J20/28B01D53/22B01D53/02
CPCB01D67/0002B01D67/0006B01D69/12B01D69/02B01J20/226B01J20/28033B01D53/228B01D53/02B01J2220/4806B01J2220/4812
Inventor魏昕郦和生孟凡宁王成鸿侯秀华
OwnerCHINA PETROLEUM & CHEM CORP