Preparation method of metal organic framework membrane for CO2 separation

A metal-organic framework and seed crystal technology, applied in separation methods, semi-permeable membrane separation, dispersed particle separation, etc., can solve the problems that are not conducive to membrane adhesion, and achieve the effect of wide film-forming conditions and good performance

Active Publication Date: 2013-12-25
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, compared with the sheet-like support, the special force field brought by its geometric shape is not conducive to the attac

Method used

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  • Preparation method of metal organic framework membrane for CO2 separation
  • Preparation method of metal organic framework membrane for CO2 separation
  • Preparation method of metal organic framework membrane for CO2 separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 Preparation of Metal-Organic Framework Membrane-CAU-1 Membrane by Single-Solvent Secondary Seeding Method

[0034] (1) Preparation of seed crystals: AlCl 3 ·6H 2 O (2.261g, 9.36mmol), H 2 N-H 2 Mix BDC (0.568g, 3.14mmol) and methanol (30mL) evenly, ultrasonically oscillate until the solid is completely dissolved, put it into a polytetrafluoro-lined stainless steel kettle, react at 125°C for 5h, and centrifuge at 10,000rpm for 10min after the reaction is completed , remove the supernatant, and wash the lower layer with deionized water first (every 0.5g of the lower layer is dispersed in 2000ml of deionized water) for 12h, then stir and wash with methanol (every 0.5g of the lower layer is dispersed in 500ml of methanol) for 12h, and wash away unreacted The components of the reaction solution were vacuum-dried at 100°C for 3 days to obtain CAU-1 seed crystals.

[0035] The synthesized CAU-1 crystals were subjected to XRD ( figure 1 ) and SEM ( figure 2 ) r...

Embodiment 2

[0042] Example 2 Preparation of Metal Organic Framework Membrane-CAU-1 Membrane by Mixed Solvent Secondary Seeding Method

[0043] The carrier tube coated with the seed crystal was prepared according to the method of (1)-(3) in Example 1.

[0044] AlCl 3 ·6H 2 O (1.01g, 4.18mmol) and H 2 N-H 2 BDC (0.25g, 1.38mmol) was dissolved in a mixed solution of 20ml of methanol and ethanol (the volume ratio of methanol and ethanol was 1:2) by ultrasonic vibration to configure the film-forming solution. Transfer the film-forming solution into a stainless steel kettle lined with PTFE, and at the same time put the prepared pre-coated carrier tube with seed crystals vertically into the kettle to ensure that the film-forming solution covers the carrier tube and seal the The reaction kettle was placed in an oven at 125°C for 12 hours, and the carrier tube was stirred and washed with methanol for 5 times. membrane.

[0045] Mixed gas test: put the synthesized metal-organic framework memb...

Embodiment 3

[0049] Example 3 Preparation of Metal Organic Framework Membrane-CAU-1 Membrane by Mixed Solvent In-situ Growth Method

[0050] The α-Al2O3 carrier tube was prepared according to the method in (2) of Example 1 for future use.

[0051] AlCl 3 ·6H 2 O (1.01g, 4.18mmol) and H 2 N-H 2 BDC (0.25g, 1.38mmol) was dissolved in a mixed solution of 20ml of methanol and ethanol (the volume ratio of methanol and ethanol was 1:2) by ultrasonic vibration to configure the film-forming solution. Transfer the film-forming solution into a stainless steel kettle lined with polytetrafluoroethylene, and at the same time put the prepared α-Al 2 o 3 Put the carrier tube vertically into the kettle, make sure that the film-forming solution covers the carrier tube, put the closed reaction kettle in an oven at 125°C for 12 hours, stir and wash the carrier tube with methanol for 5 times, the first two times are 5 hours, and then Wash for 12 hours each time three times, and then dry in a vacuum oven...

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Abstract

The present invention discloses a preparation method and an application of a metal organic framework membrane for CO2 separation. The metal organic framework membrane preparation method comprises: dissolving AlCl3.6H2O and H2N-H2BDC in methanol or a methanol and solution A mixed solution to prepare a membrane forming solution; and placing a carrier with CAU-1 crystal seed introduction or with no crystal seed introduction in the prepared membrane forming solution, making the membrane forming solution be subjected to crystallization membrane forming on the surface of the carrier, washing, and drying. The metal organic framework membrane is the first novel MOF membrane material capable of effectively separating CO2 and N2 under the flue channel gas composition condition, wherein the membrane forming condition is broad, and the continuous membrane layer can be formed with the in situ growth method, the secondary crystal seed method and the internal and external diffusion method. The membrane presents good performances in applications of separation of CO2/N2 and CO2/CH4 in flue gas and nature gas.

Description

technical field [0001] The invention belongs to the technical field of new materials, and relates to a preparation method of a dense continuous microporous ammonia-functionalized aluminum-containing metal-organic framework compound (metal organic frameworks, MOFs) membrane-CAU-1 membrane and its use in the production of flue gas Separation of CO from natural gas 2 in the application. Background technique [0002] CO released from flue gas or natural gas 2 Considered to be one of the major contributors to global warming, CO 2 The development of advanced materials and technologies for capture plays a very important role in the sustainable development of society and economy. At present, most of the commercial use of amino-functionalized materials through the adsorption process for CO 2 For capture, as opposed to the use of membrane technology for adsorption and separation to capture CO 2 is a better choice. [0003] Membrane components are the core of membrane separation ...

Claims

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Application Information

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IPC IPC(8): B01D71/06B01D69/10B01D67/00B01D53/22
CPCY02C20/40
Inventor 杨建华殷慧敏王金渠谢忠白菊鲁金明张艳殷德宏
Owner DALIAN UNIV OF TECH
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