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Preparation method of pervaporation metal organic framework UiO-66 series gasoline desulfurization film

A metal-organic framework and pervaporation technology, applied in chemical instruments and methods, semi-permeable membrane separation, refining by dialysis, etc., can solve the problems of harsh film forming conditions, harsh membrane synthesis conditions, and affecting separation performance, and achieve high performance Stable, good repeatability and stability, excellent performance

Active Publication Date: 2018-05-15
DALIAN UNIV OF TECH
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AI Technical Summary

Problems solved by technology

However, due to the harsh synthesis conditions of UiO-66 series membranes, there are few reports at present. The current synthesis methods include in-situ methods [Liu X L, Demir N K, Wu Z T, et al. Highly Water-Stable Zirconium Metal-Organic framework UiO-66 membranes supported on aluminum hollow fibers for desalination[J].Journal of the American Chemical Society.2015,137(22):6999-7002], secondary seed crystal method[F.C.Wu,L.Lu,H.O.Liu,et al.Synthesis of stable UiO-66membranes for permeability separation of methanol / methyl tert-butyl ethermixtures by secondary growth.Journal of membrane science.Doi.org / 10.1016 / j.memsci.2017.09.047.], chemical modification [Wan L L, Zhou.C. , Xu.K, et al.Synthesis of highly stable UiO-66-NH 2 membranes with high ions rejection for seawater desalination. Microporous and Mesoporous Materials. 2017(252):207-213]
Although the above methods have obtained dense films, there are certain problems: the in-situ method is easy to operate, but due to the low nucleation density of MOFs support, it is difficult to prepare, and the film-forming conditions of UiO-66 film are relatively harsh. , so the success rate of the in-situ method is low; the seed method overcomes the shortcomings of the in-situ method to a certain extent, but the bonding force between the film layer and the carrier is poor. In addition, in the preparation of UiO-66 film, the seed method The obtained film layer must be thicker to reverse the defects caused by the growth characteristics of the film, but the thicker film layer greatly affects its separation performance; the chemical modification method has certain limitations, and the method in the prior art needs to grow two times to get UiO-66-NH 2 film layer, the complex and cumbersome film-making process greatly reduces its film-forming efficiency
[0004] In summary, the preparation of UiO-66 series membranes is difficult at present, and there are certain problems in the existing preparation methods.

Method used

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  • Preparation method of pervaporation metal organic framework UiO-66 series gasoline desulfurization film
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  • Preparation method of pervaporation metal organic framework UiO-66 series gasoline desulfurization film

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Experimental program
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Effect test

Embodiment 1

[0017] Preparation of UiO-66 film

[0018] (1) Carrier pretreatment:

[0019] α-Al with a pore size of 0.2 μm 2 o 3 The ceramic tube carrier was vibrated in ultrasonic with acetone and ethanol, then rinsed with deionized water several times, vibrated ultrasonically, and dried at 100°C for later use.

[0020] (2) The inner surface of the carrier is introduced into the zirconia sol layer

[0021] Dissolve 10g of zirconia octahydrate into 50mL of ethanol, stir vigorously at room temperature and add concentrated hydrochloric acid dropwise to adjust the pH to 2.0 to avoid precipitation, stir at room temperature for 12h, and then age for 24h to obtain a colorless and transparent zirconia sol; The rubber-tipped pipette sucks the zirconia sol and adds it to the α-Al 2 o 3 In the ceramic tube carrier, hover and pull for 20s, the thickness of the zirconia sol layer is about 1μm, dry at 60°C for 12h, and then bake in a muffle furnace at 400°C for 4h, with a heating and cooling rate ...

Embodiment 2

[0027] UiO-66-NH 2 Membrane preparation

[0028] (1) Carrier pretreatment:

[0029] Macroporous α-Al with a pore size of 1-3 μm 2 o 3 The ceramic tube carrier was vibrated in ultrasonic with acetone and ethanol, then rinsed with deionized water several times, vibrated ultrasonically, and dried at 100°C for later use.

[0030] (2) Zirconia sol layer is introduced into the inner surface of alumina carrier

[0031]Dissolve 10g of zirconia octahydrate into 50mL of ethanol, stir vigorously at room temperature and add concentrated hydrochloric acid dropwise to pH 2.0 to avoid precipitation, stir at room temperature for 12h, and then age for 24h to obtain a colorless and transparent zirconia sol; The zirconia sol was sucked into the alumina tube with the suction pipe, hovered and pulled for 20s, the thickness of the zirconia sol layer was about 1 μm, dried at 60°C for 12h, and then baked in a muffle furnace at 400°C for 4h, the heating and cooling rates were uniform. 1°C / min.

...

Embodiment 3

[0037] Preparation of mixed ligand membranes

[0038] (1) Carrier pretreatment:

[0039] α-Al with a pore size of 0.2 μm 2 o 3 The ceramic tube carrier was vibrated in ultrasonic with acetone and ethanol, then rinsed with deionized water several times, vibrated ultrasonically, and dried at 100°C for later use.

[0040] (2) The inner surface of the carrier is introduced into the zirconia sol layer

[0041] Dissolve 10g of zirconia octahydrate into 50mL of ethanol, stir vigorously at room temperature and add concentrated hydrochloric acid dropwise to adjust the pH to 2.0 to avoid precipitation, stir at room temperature for 12h, and then age for 24h to obtain a colorless and transparent zirconia sol; The rubber-tipped pipette sucks the zirconia sol and adds it to the α-Al 2 o 3 In the ceramic tube carrier, hover for 20s, dry at 80°C for 10h, and then bake in a muffle furnace at 400°C for 4h, with a heating and cooling rate of 1°C / min.

[0042] (3) Preparation of double-liga...

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Abstract

A preparation method of a pervaporation metal organic framework UiO-66 series gasoline desulfurization film includes: introducing a zirconia sol layer firmly combined with a carrier onto the carrier to obtain the carrier with the zirconia sol layer, and performing solvothermal growing to prepare a film layer; in the process of growing, the zirconia sol layer provides a metal source for a Uio-66 series film and serves as a active site and a connection point of film forming to promote forming of the UiO-66 series film which is continuous, uniform and complete. The UiO-66 series film prepared bythe method is a hydrophilic film and can preferentially adsorb thiophene with relatively high polarity; zirconium in a framework of the UiO-66 series film has special adsorption effect on thiophene, so that the UiO-66 series film has excellent performance in pervaporation dulsufurization, enrichment factor is higher than 10, and permeation flux is greater than 1.0kgm-2h-1. In addition, UiO-66 series materials are comparatively stable, so that the obtained film can be operated continuously for a long time (longer than 3d) while maintains stable performance.

Description

technical field [0001] The invention belongs to the field of preparation of metal-organic framework membranes, and in particular relates to a method for preparing metal-organic UiO-66 series membranes through in-situ direct transformation of a zirconia sol layer. Background technique [0002] Sulfur compounds in gasoline are one of the main causes of air pollution. Countries around the world have successively promulgated more and more stringent regulations to control the sulfur content in gasoline, and gasoline deep desulfurization technology has become a research hotspot. Membrane pervaporation gasoline desulfurization technology is a new type of gasoline desulfurization technology, which has the advantages of low investment and operating costs, modular design, easy expansion and construction, and has attracted extensive attention from the petrochemical industry. At present, the membrane materials used in pervaporation gasoline desulfurization are mainly organic membranes. ...

Claims

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Application Information

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IPC IPC(8): B01D71/06B01D67/00B01D61/36C10G31/11
Inventor 张雄福吴飞超刘海鸥
Owner DALIAN UNIV OF TECH
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