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MOFs material-based series molecular sieve and preparation method and application method thereof in complex sample purification and separation analysis

A molecular sieve and micro-injector technology, which is used in solid-phase microextraction and chromatography applications, can solve the problem that the size selectivity of MOFs material-based molecular sieve materials is not fully exerted, there is no analysis, and the chromatographic column cannot effectively reflect the selectivity, etc. It is beneficial to large-scale promotion and application, easy to manufacture, and has great practical significance for production.

Inactive Publication Date: 2011-06-15
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

None of the above chromatographic columns can effectively reflect the selectivity in the separation process
[0006] At present, the research on using MOFs materials as solid-phase microextraction coatings and chromatographic stationary phases is still in its infancy. However, most of the existing studies have not fully utilized the size selectivity of MOFs materials as a class of molecular sieve materials, and there is currently no Apply it to the analysis of actual complex samples

Method used

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  • MOFs material-based series molecular sieve and preparation method and application method thereof in complex sample purification and separation analysis
  • MOFs material-based series molecular sieve and preparation method and application method thereof in complex sample purification and separation analysis
  • MOFs material-based series molecular sieve and preparation method and application method thereof in complex sample purification and separation analysis

Examples

Experimental program
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Embodiment 1

[0048] (a) Preparation of fiber extraction head coated with metal-organic porous framework material MOF-199

[0049] First, the pretreatment of stainless steel fibers:

[0050] Put a stainless steel fiber with an outer diameter of 0.15mm and a total length of 17cm with a length of 3.0cm in aqua regia, and corrode it at room temperature for 40 minutes. By controlling the corrosion time, the outer diameter of the stainless steel fiber is controlled so that the outer diameter of the stainless steel fiber after corrosion is 0.05. mm, rinsed with pure water and dried.

[0051] Second, the metal-organic porous framework material coating is prepared by layer-by-layer coating method on the surface of stainless steel fibers:

[0052] Put 24mL of water, methanol and N,N-dimethylformamide in a single-necked bottle with a volume ratio of 1:1:1, and 1mmol Cu(OAc) 2 ·H 2 O and 0.6 mmol 1,3,5-benzenetricarboxylic acid were dissolved in a one-necked flask, and after the solution was mixed,...

Embodiment 2

[0057] (a) Preparation of fiber extraction head coated with metal-organic porous framework material ZIF-8

[0058] First, the pretreatment of stainless steel fibers:

[0059] Put a stainless steel fiber with an outer diameter of 0.25mm and a total length of 18cm with a length of 4.0cm in aqua regia, and corrode it at room temperature for 30 minutes, and control the outer diameter of the stainless steel fiber by controlling the corrosion time, so that the outer diameter of the stainless steel wire after corrosion is 0.15mm , rinse with pure water and dry.

[0060] Second, the metal-organic porous framework material coating is prepared by layer-by-layer coating method on the surface of stainless steel fibers:

[0061] Put 40mL of methanol solvent in a single-necked bottle, mix 1mmol Zn(NO 3 ) 2 ·6H 2 O and 8 mmol 2-methylimidazole were dissolved in a single-necked bottle, and after the solution was mixed, the reaction was stirred at room temperature for 1 hour. After the re...

Embodiment 3

[0066] (a) Preparation of fiber extraction head coated with metal-organic porous framework material ZIF-7

[0067] First, the pretreatment of stainless steel fibers:

[0068] Put a 0.15mm outer diameter and 16cm long stainless steel fiber with a length of 2.5cm in aqua regia, and corrode it at room temperature for 25 minutes. Control the outer diameter of the stainless steel fiber by controlling the corrosion time, so that the outer diameter of the stainless steel wire after corrosion is 0.10mm , rinse with pure water and dry.

[0069] Second, the metal-organic porous framework material coating is prepared by layer-by-layer coating method on the surface of stainless steel fibers:

[0070] Put 100mL of methanol solvent in a single-necked bottle, mix 1mmol Zn(NO 3 ) 2 ·6H 2 O and 6.5 mmol of phenylimidazole were dissolved in a single-necked bottle, and after the solution was mixed, the reaction was stirred at room temperature for 48 hours. After the reaction is finished, the ...

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Abstract

The invention discloses a metal-organic frameworks (MOFs) material-based series molecular sieve and a preparation method and an application method thereof in complex sample purification and separation analysis, and relates to the technical field of chromatography application and the field of solid phase micro extraction. The series molecular sieve comprises an MOFs material-based solid phase micro extraction device and an MOFs material-based capillary gas phase chromatographic column; the MOFs material-based solid phase micro extraction device comprises a section of stainless steel fiber extraction head, the surface of which is coated with an MOFs material; and the MOFs material-based capillary gas phase chromatographic column comprises a section of capillary, the inner wall of which is uniformly coated with a layer of MOFs material. High-selectivity purification, efficient separation and specificity detection and measurement of a complex sample are realized by combined use of the solid phase micro extraction device coated with the MOFs material and the gas phase chromatographic column coated with the MOFs material. The series molecular sieve is favorable for large-scale popularization and application, and has broad application prospect in the fields of analytical chemistry, particularly environmental analysis, food analysis and the like.

Description

technical field [0001] The invention relates to the technical field of chromatographic application and the technical field of solid-phase microextraction, in particular to a serial molecular sieve based on MOFs material. Background technique [0002] Metal-Organic Frameworks (MOFs) materials, also known as coordination polymers (Coordination Polymers) materials, are a class of molecular sieve-like porous materials based on the interaction between metals and organic ligands. The formation of such substances is usually a self-assembly process of metals and organic ligands. Metals provide empty orbitals as electron acceptors, and atoms such as nitrogen and oxygen in the ligands provide electron pairs as electron donors. It is precisely because of the introduction of organic ligands into MOFs materials that it becomes possible in the directional synthesis and material directional design of such porous materials. The size of the pores can be controlled by adjusting the size of th...

Claims

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Application Information

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IPC IPC(8): B01J20/281G01N30/02
CPCB01J20/282B01J2220/86B01J20/226
Inventor 严秀平常娜王荷芳
Owner NANKAI UNIV
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