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Organic metal framework material mixed matrix membrane and preparation method thereof

A technology of mixed matrix membranes and skeleton materials, applied in the field of membrane materials, to achieve low cost, various specifications, and reduce the loss of adsorbents

Inactive Publication Date: 2021-07-09
佛山市南海区苏科大环境研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, MOF-MMMs are mainly used in gas phase separation, nanoscale filtration, molecular sieving and catalysis, and are rarely used in solid phase extraction.

Method used

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  • Organic metal framework material mixed matrix membrane and preparation method thereof
  • Organic metal framework material mixed matrix membrane and preparation method thereof
  • Organic metal framework material mixed matrix membrane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation method of the UiO-66(Zr)-MMMs mixed matrix membrane of the present embodiment adopts the following steps:

[0035] 1) UiO-66(Zr): Mix zirconium chloride (0.318g) and terephthalic acid (0.204g) with 40mL DMF, stir it magnetically for 10min, then put it in an autoclave and react at 120°C 24h. After cooling, the mixture was soaked in 50 mL DMF for 30 min, centrifuged at 8000 rpm for 5 min to collect the solid product, washed three times with ultrapure water and ethanol, and then vacuum-dried at 60 °C for 10 h to obtain a white powder. This embodiment should have the following features: the X-ray diffraction results show the characteristic peaks of UiO-66(Zr) near the positions of θ=7.3°, 8.4°, 25.7°, etc., and UiO-66(Zr) is formed into a film , still retains a certain crystal structure; Fourier transform infrared spectrum at 1568, 1020, 742, 665 and 1180cm -1 There are characteristic absorption peaks nearby.

Embodiment 2

[0037] The MIL-53(Al)-MMMs mixed matrix membrane preparation method of this embodiment adopts the following steps:

[0038]1) MIL-53(Al): Disperse 3.38g of aluminum nitrate nonahydrate and 1.00g of terephthalic acid in a mixed solution of 44mL DMF and 16mL of ultrapure water, and mechanically stir in a water bath at 40°C for 2h . The mixture was transferred to an autoclave with a volume of 100 mL, and then reacted in an oven at 130° C. for 48 h. After cooling, the mixture was soaked in 50 mL of DMF for 30 min, centrifuged at 8000 rpm for 5 min to collect the solid product, washed three times with ultrapure water and ethanol, and then vacuum-dried at 60°C for 10 h to obtain a white powder.

Embodiment 3

[0040] NH in this example 2 -MIL-101 (Fe)-MMMs mixed matrix film preparation method, adopts the following steps:

[0041] 1) NH 2 -MIL-101(Fe): Preparation of NH using solvothermal method 2 -MIL-101(Fe). Ferric chloride hexahydrate (19.75 mmol, 5.338 g) and terephthalic acid (10.0 mmol, 1.812 g) were added to 60 mL of DMF solution, and the mixture was magnetically stirred for 10 min, and then transferred to a 100 mL polytetrafluoroethylene liner in a stainless steel autoclave and heated at 110°C for 24h. After cooling, the mixture was soaked in 50 mL of DMF for 30 min, centrifuged at 8000 rpm for 5 min to collect the solid product, washed three times with ultrapure water and ethanol, and then vacuum-dried at 60 °C for 10 h to obtain a dark brown solid powder.

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Abstract

The invention discloses a method for detecting PAHs in tea soup by combining an injector type membrane microextraction technology based on a metal organic framework-mixed matrix membrane (MOF-MMM) with an HPLC method (SMME / HPLC-FLD). According to the invention, four kinds of MOF-MMM are prepared, namely, UiO-66 (Zr)-MMM, MIL-53 (Al)-MMM, MIL-101-MMM and NH2-MIL-101-MMM are prepared, MOF-MMM with the diameter of 25 mm is sheared and put into a replaceable membrane filter head, and then a simple extraction device can be assembled by virtue of a needle cylinder. In the enrichment and extraction process, benzene rings in the MOFs are combined with the PAHs through pi-pi interaction and / or hydrophobic interaction, and efficient separation and enrichment of the PAHs in the tea soup are achieved. The injector type membrane microextraction device has the advantages of convenience in carrying, simplicity in operation, low cost and the like; meanwhile, the UiO-66 (Zr)-MMM can simply and rapidly enrich PAHs in the process of being in contact with the sample, vortex or ultrasound is not needed in the adsorption process, and after adsorption, the adsorbed MOFs particles do not need to be collected through centrifugation. The method is very suitable for analysis and detection of trace PAHs in food samples.

Description

technical field [0001] The invention belongs to the field of membrane materials, and in particular relates to an organometallic framework material mixed matrix membrane and a preparation method. Background technique [0002] In recent years, the development of some green and environment-friendly pretreatment technologies that do not use or use less organic solvents has become the main research direction in the field of analytical chemistry. Among them, the solid-phase extraction technology using metal-organic frameworks (MOFs) as adsorbents is becoming more and more mature. MOFs are a new class of porous materials. They are usually porous crystals with an infinitely expanding network structure formed by the hybridization of inorganic metal ions and organic ligands. Due to the diversity of their structures and properties, MOFs are widely used in many fields, such as catalysis, gas separation and storage, sensors, nonlinear optical drug delivery, and removal of organic matter...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/08
CPCB01J20/265B01J20/226B01J20/28033B01D15/08
Inventor 高明王学东王慧利张薇
Owner 佛山市南海区苏科大环境研究院
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