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A capillary monolithic column for separation of benzene homologues and preparation method thereof

A technology of capillary monolithic columns and homologues, which is applied in the fields of analytical chemistry and environmental analysis, can solve problems such as difficult and efficient use of MOFs materials, and achieve good stability and good separation effect

Active Publication Date: 2021-11-19
HUBEI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are several problems in this method of embedding MOFs materials: First, due to the high surface energy and strong van der Waals force of MOFs materials, MOFs materials are prone to aggregation and separation.
Secondly, with the embedding method, most of the MOFs materials will be wrapped into the aggregated particles of the monolithic column, which makes it difficult to efficiently utilize the unique properties of MOFs materials

Method used

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  • A capillary monolithic column for separation of benzene homologues and preparation method thereof
  • A capillary monolithic column for separation of benzene homologues and preparation method thereof
  • A capillary monolithic column for separation of benzene homologues and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 Preparation of a capillary monolithic column for the separation of benzene homologues

[0024] 1. Synthesis of MOF-5:

[0025] 1. Using the classic hot solvent method, a certain amount of Zn(NO 3 ) 2 ·6H 2 O and H 2 BDC (terephthalic acid) is mixed, dissolved in an appropriate amount of DMF, shaken vigorously for 30 minutes and placed in a high-temperature and high-pressure reactor. After reacting at 120°C for 24 hours, the product was suction-filtered and washed three times with DMF, each time 15 mL, to remove unreacted reactants. Use CH again 2 Cl 2 (dichloromethane) for one day to remove the DMF in the guest molecule. Finally, the prepared MOF-5 was vacuum-dried at 120°C for 24 hours to obtain a white solid, which was characterized by XRD, SEM, and infrared.

[0026] Table 1 raw material consumption

[0027]

[0028] 2. The XRD spectrum of the prepared MOF-5 material is as follows figure 2 shown. It can be seen from the figure that the charac...

experiment example 1

[0044] Experimental example 1 Stability analysis of a capillary monolithic column used for separation of benzene homologues

[0045] When methanol is used as the mobile phase, the flow rate is from 0.02mL·min -1 to 0.06mL·min -1 There is a nice linear relationship between back pressure and flow rate, indicating that the permeability does not change with flow rate as in Image 6 shown. When water is used as the mobile phase, the flow rate and back pressure also have a linear relationship and the R value reaches 0.99. Figure 7 shown. Bring the data into the permeability formula to calculate the permeability K as the following table:

[0046] Table 4-Physical data of each substance

[0047]

experiment example 2

[0048] Experimental example 2 detects the separation effect of homologues of benzene

[0049] 1. Connect the monolithic capillary column MOF-5@ploy(GMA-co-EDMA) (experimental group) and monolithic capillary column poly(GMA-co-EDMA) (control group) to HPLC (FL2200) respectively. The mobile phase was 75% methanol / 25% water, and the ultraviolet spectrum was used as the detector, and the flow rate was 0.02mL·min-1. Take 10 microliters each of 1% toluene (methanol:toluene=99:1, v / v), 1% benzene (methanol:benzene=99:1, v / v), 0.5% phenol (MeOH:Phenol=199: 1, v / v) Shake well in a centrifuge tube. Inject 20 μL of the mixed solution with a sampler and detect it with a 245nm ultraviolet detector.

[0050] 2. If Figure 8 As shown, the GMA-EDMA monolithic column without immobilized MOF-5 (control group) did not have any separation ability for the mixed solution, and only one peak appeared.

[0051] 3. If Figure 9 As shown, the monolithic column (experimental group) of immobilized MO...

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Abstract

The invention discloses a capillary monolithic column for the separation of benzene homologues and a preparation method thereof. The mixed liquid obtained by dissolving GCC in ethanol is added into a sample bottle equipped with MOF-5 according to a certain amount, and the obtained suspended The liquid is injected into the ploy (GMA-co-EDMA) monolithic post activated by ethylenediamine to obtain the capillary monolithic column MOF-5@ploy (GMA-co-EDMA); the present invention uses the surface covalent immobilization method to MOF‑5 is immobilized on the surface of GMA‑EDMA monolithic column, MOF‑5 is dispersed in a mixture of DCC and ethanol, and the epoxy functional groups on the surface of polymethacrylate (PMMA) are opened by ethylenediamine to make MOF‑5 covalent Immobilized on the surface of the polymer in the monolithic column, since MOF-5 is covalently connected to the monolithic column, it will not cause aggregation and separation of MOFs materials, and the properties of MOFs materials will not be greatly affected.

Description

technical field [0001] The invention relates to the technical fields of analytical chemistry and environmental analysis, in particular to a capillary integral column for separating benzene homologues and a preparation method thereof. Background technique [0002] Solid phase microextraction (SPME) is a new type of sample pretreatment technology, which was first proposed by the Pawliszyn research group in Canada in 1989. This technology integrates sampling, extraction, enrichment and sample injection, does not consume solvents, and can be used online with other instruments. It has developed rapidly in less than 20 years, and various types of extraction media have emerged continuously. . The basic principle of SPME is to immobilize the coating material with adsorption function on the surface of a certain matrix fiber by physical or chemical methods, make direct or indirect contact with the sample, enrich and concentrate the target analyte, and combine it with The sample inje...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/10
CPCB01D15/10
Inventor 吴帅宾谢一铭
Owner HUBEI NORMAL UNIV
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