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Preparation method and application of metal organic framework (MOF)-derived magnetic porous carbon material

A porous carbon material and magnetic technology, applied in the direction of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problems of limited application, easy collapse, etc., achieve good stability, increase ratio The best surface area and adsorption performance

Pending Publication Date: 2020-04-10
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the structure of most MOFs materials is easy to collapse in water, which limits their application in the field of sample pretreatment.

Method used

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  • Preparation method and application of metal organic framework (MOF)-derived magnetic porous carbon material
  • Preparation method and application of metal organic framework (MOF)-derived magnetic porous carbon material
  • Preparation method and application of metal organic framework (MOF)-derived magnetic porous carbon material

Examples

Experimental program
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Effect test

Embodiment 1

[0036] This embodiment provides the preparation method of MOFs derived magnetic porous carbon material MPCK, including the following steps: Weigh 3.2 gFeCl 3 •6H 2 O and 1.0 g of PTA were dissolved in 70 mL of DMF, and after complete dissolution, they were transferred to a 100 mL hydrothermal reaction synthesis kettle, sealed and placed in an oven at 110 °C for 24 h. Cool to room temperature, wash with DMF and acetone, and dry under vacuum at 60 °C for 8 h to obtain orange solid MIL-101(Fe). Weigh 0.4 g KOH and 0.2 g MIL-101(Fe) into a porcelain boat, then put them into a high-temperature combustion tube furnace, carbonize at 700 °C for 4 h, let it cool naturally, and adjust with 0.1 mol / L HCl pH to neutral, and then washed with deionized water to obtain MOFs-derived magnetic porous carbon material MPCK.

[0037] Below, the physical and chemical properties of MPCK are characterized by FT-IR and SEM.

[0038] Depend on figure 1 As shown in a, at 748 cm -1 The peak at is a...

Embodiment 2

[0041] In this embodiment, the method for preparing MOFs-derived magnetic porous carbon material MPCK using Example 1 includes the following steps:

[0042] The effect of the ratio of KOH solid to MIL-101(Fe) on the yield of MPCK was investigated.

[0043]MPCK was prepared according to the method described in Example 1, with the difference that the ratios of KOH solid to MIL-101(Fe) were 1:1, 2:1, and 3:1, respectively. As can be seen from the observation results, when the ratio is 1:1, MPCK is not completely carbonized; when the ratio is 3:1, the yield of MPCK drops significantly; when the ratio of KOH solid to MIL-101(Fe) is 2:1, The yield of MPCK is the largest and the carbonization is complete, so the ratio selected by the present invention is 2:1.

Embodiment 3

[0045] The present embodiment utilizes carmine and amaranth in the MPCK extraction aqueous solution that embodiment 1 prepares, comprises the following steps:

[0046] The influence of the quality of MPCK on the extraction efficiency was investigated.

[0047] Pipette 100 μL of the mixed standard with a concentration of 5 mg / L, add it into a brown sample bottle, and dilute to 10 mL with deionized aqueous solution with pH=7. The amount of MOFs-derived magnetic porous carbon material MPCK added is 3 mg, 5 mg, 10 mg, 20 mg, vortex extraction for 20 min, magnetic separation, discard the supernatant, add 3 mL (ammonia:methanol=2%:98%) eluent; vortex elution for 20 min, magnetic separation , the eluent was blown dry with nitrogen gas, fixed to volume with mobile phase, centrifuged at 12000 r / min for 10 min, and the supernatant was removed for chromatographic analysis. Depend on image 3 It can be seen that when the mass of the adsorbent reaches 5 mg, the extraction efficiency reac...

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Abstract

The invention discloses an MOF-derived magnetic porous carbon material and a method for extracting dyes (amaranth and carmine) by using the material. The preparation method comprises the following steps: with FeCl3.6H2O and p-phthalic acid (PTA) as raw materials, preparing a metal organic framework MIL-101 (Fe); and then with the MIL-101 (Fe) as a raw material and KOH as an activating agent, carrying out high-temperature calcination under the protection of N2 to prepare the MOF-derived magnetic porous carbon material (MPCK). The MPCK can be used as a magnetic adsorbent for extracting carmine and amaranth in a beverage, and sensitive detection of a target analyte is realized through combination of the MPCK and high performance liquid chromatography.

Description

technical field [0001] The invention belongs to the technical field of carbon-based composite materials, and in particular relates to the preparation of a MOFs-derived magnetic porous carbon material, which can be applied to the extraction of carmine and amaranth in aqueous solution, and further applied to the determination of carmine and amaranth in beverages . Background technique [0002] Food colorings, also known as food dyes, are often used as food additives to improve sensory properties. Food dyes can be divided into two categories, namely natural food dyes and synthetic food dyes. Among them, natural food dyes are dyes directly extracted from animal and plant tissues, which are generally harmless to the human body; while synthetic food dyes are made from aniline dyes separated from coal tar, so they are also called Coal tar pigments or aniline pigments, such as synthetic amaranth, carmine, etc. These synthetic dyes are harmful to the human body because they are ea...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/28B01J20/30C02F1/28C02F101/30C02F101/38
CPCB01J20/20B01J20/28009B01J20/28057C02F1/281C02F1/283C02F2101/308C02F2101/38
Inventor 连丽丽张鑫洋娄大伟王希越张浩祝波刘立业
Owner JILIN INST OF CHEM TECH
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