Preparation and application of hollow zirconium-based porphyrin type metal organic framework solid-phase microextraction fiber

A metal-organic framework and zirconium-based porphyrin-based technology, applied in fiber treatment, alkali metal compounds, alkali metal oxides/hydroxides, etc., can solve problems such as single microporous structure, difficult macromolecules, mass transfer limitations, etc. , to achieve the effect of fast mass transfer rate, high utilization of specific surface area, and overcoming thermal instability

CN113893835AActive Publication Date: 2022-01-07FUZHOU UNIV
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2022-01-07

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Abstract

The invention discloses a method for preparing a solid-phase microextraction fiber with a hollow zirconium-based porphyrin type metal organic framework material as a coating based on an in-situ growth method, and belongs to the field of solid-phase microextraction fiber preparation. The solid-phase microextraction fiber is prepared by taking a stainless steel fiber modified by polydopamine as a matrix and taking zircon salt, benzoic acid, meso-tetra(4-carboxyphenyl)porphin and water as raw materials, and can be used for detecting 1-naphthol and 2-naphthol. The prepared hollow zirconium-based porphyrin type metal organic framework material is good in thermal stability, rich in adsorption active sites and large in specific surface area, solid-phase microextraction fibers prepared from the hollow zirconium-based porphyrin type metal organic framework material are good in reproducibility and long in service life, and 1-naphthol and 2-naphthol in a complex matrix can be measured at the same time through the established method.
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Description

technical field

[0001] The invention belongs to the field of solid-phase microextraction fiber preparation, in particular to a preparation method of a solid-phase microextraction fiber coated with a hollow zirconium-based porphyrin type metal-organic framework material and its application in 1-naphthol and 2-naphthol application in extraction. Background technique

[0002] 1-naphthol and 2-naphthol are two common industrial raw materials, which are widely used in the production of oils, dyes, spices, pesticides, drugs, etc. Both 1-naphthol and 2-naphthol are considered to be highly toxic environmental pollutants, which can reduce human semen quality and testosterone levels, and even cause severe systemic poisoning. Due to the wide range of applications, naphthol will inevitably be released and exposed to the ecological environment. Therefore, it is particularly important to detect 1-naphthol and 2-naphthol in the environment. However, due to the low content of naphthol in...

Examples

Embodiment 1

[0029] 1) Preparation of polydopamine-modified stainless steel fibers:

[0030] a. Soak the 3cm-long end of the stainless steel fiber in hydrofluoric acid at 70°C for 15 minutes, then ultrasonically clean it with pure water to obtain a stainless steel fiber with a rough surface at one end, and dry it for later use;

[0031] b. Put the treated end of the stainless steel fiber in 2 mg·mL -1 Dopamine aqueous solution, and adjust its pH value to 8.5 with Tris-HCl solution, and leave it at room temperature for 24 h to obtain PDA-modified stainless steel fibers;

[0032] 2) Preparation of HZP-MOFs solid-phase microextraction fibers:

[0033] c. Dissolve 10 mg zirconium chloride, 200 mg benzoic acid and 200 μl water in 2 mL DMF, stir at room temperature for 5 minutes, then add 10 mg TCCP, and continue stirring for 10 minutes to obtain a homogeneous solution;

[0034] d. Transfer the obtained homogeneous solution to a 12 mL autoclave, immerse the prepared polydopamine-modified stain...

Embodiment 2

[0039] 1) Preparation of polydopamine-modified stainless steel fibers:

[0040] a. Soak the 3cm-long end of the stainless steel fiber in hydrofluoric acid at 70°C for 15 minutes, then ultrasonically clean it with pure water to obtain a stainless steel fiber with a rough surface at one end, and dry it for later use;

[0041] b. Put the treated end of the stainless steel fiber in 2 mg·mL -1 Dopamine aqueous solution, and adjust its pH value to 8.5 with Tris-HCl solution, and leave it at room temperature for 24 h to obtain PDA-modified stainless steel fibers;

[0042] 2) Preparation of HZP-MOFs solid-phase microextraction fibers:

[0043] c. Dissolve 10 mg zirconium chloride, 250 mg benzoic acid and 200 μl water in 2 mL DMF, stir at room temperature for 5 minutes, then add 10 mg TCCP, and continue stirring for 10 minutes to obtain a homogeneous solution;

[0044] d. Transfer the obtained homogeneous solution to a 12 mL autoclave, immerse the prepared polydopamine-modified stain...

Embodiment 3

[0046] 1) Preparation of polydopamine-modified stainless steel fibers:

[0047] a. Soak the 3cm-long end of the stainless steel fiber in hydrofluoric acid at 70°C for 15 minutes, then ultrasonically clean it with pure water to obtain a stainless steel fiber with a rough surface at one end, and dry it for later use;

[0048] b. Put the treated end of the stainless steel fiber in 2 mg·mL -1 Dopamine aqueous solution, and adjust its pH value to 8.5 with Tris-HCl solution, and leave it at room temperature for 24 h to obtain PDA-modified stainless steel fibers;

[0049] 2) Preparation of HZP-MOFs solid-phase microextraction fibers:

[0050] c. Dissolve 10 mg of zirconium chloride, 300 mg of benzoic acid and 200 μl of water in 2 mL of DMF, stir at room temperature for 5 minutes, then add 10 mg of TCCP, and continue stirring for 10 minutes to obtain a homogeneous solution;

[0051] d. Transfer the obtained homogeneous solution to a 12 mL autoclave, immerse the prepared polydopamine...