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Preparation method and application of Fe3O4@SiO2@Zr-MOF

A reaction kettle and mixed solution technology, applied in chemical instruments and methods, other chemical processes, alkali metal oxides/hydroxides, etc., can solve rare problems, achieve good stability, good separation effect, and easy operation line effect

Inactive Publication Date: 2016-05-25
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zr-MOF has applications in gas adsorption, catalysis and other fields, but it is very rare to apply it to the adsorption of organic molecules after being combined with magnetic particles.

Method used

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  • Preparation method and application of Fe3O4@SiO2@Zr-MOF
  • Preparation method and application of Fe3O4@SiO2@Zr-MOF
  • Preparation method and application of Fe3O4@SiO2@Zr-MOF

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preparation example Construction

[0023] Fe 3 O 4 SiO 2 The preparation method of magnetic particles is as follows: ①Add 5.4g FeCl 3 ·6H 2 O, 60ml of ethylene glycol was placed in a 100ml beaker, ultrasonically stirred for 30 minutes, until a transparent solution was formed, then 3.28 sodium acetate was added, ultrasonically mixed for 30 minutes, when completely dissolved, transferred to a stainless steel kettle lined with PTFE, 200 Heated at ℃ for 10h, after cooling, collected the precipitate by magnetic separation, washed with water and ethanol under ultrasound, and dried under vacuum at 60℃ for 12h. Get Fe 3 O 4 Nano microspheres.

[0024] ②Take the new Fe 3 O 4 Add 1.0g of nanospheres to a 250ml beaker, add 200ml of 0.1mol / L hydrochloric acid, sonicate for 5min, and wash with ultrapure water 3 times. After magnetic collection, add 320ml ethanol, 80ml ultrapure water and 5ml ammonia (20% -28% mass fraction), 1ml tetraethyl orthosilicate (TEOS), and then ultrasonically shake for 10 minutes. Then transfer to a ...

Embodiment 1

[0026] Dissolve zirconium chloride (53mg) and terephthalic acid (34mg) in DMF (18mL), dissolve ultrasonically at room temperature, and then add Fe 3 O 4 SiO 2 (53mg) was then sealed in a 25mL hydrothermal reaction kettle, and then the reaction mixture was heated to 120°C, maintained at this temperature for 24h, and then cooled to room temperature. After the post-treatment, the target product was recirculated 3 times.

[0027] Fe in this example 3 O 4 SiO 2 The structure characterization and adsorption performance of Zr-MOF:

[0028] (1) Fe 3 O 4 SiO 2 Structural characterization of Zr-MOF

[0029] The D8Advance X-ray diffractometer (XRD) was used to characterize the prepared Fe3O4SiO2Zr-MOF hybrid particles. The sample is analyzed for phase and crystal form. Sample test conditions: voltage 35kV, current 20mA, 2θ scanning range is 3°~90°. And with Fe 3 O 4 The standard card is compared with the standard peak value of Zr-MOF, such as figure 1 .

[0030] The morphology and size of magn...

Embodiment 2

[0038] Dissolve 25.2mg of zirconium chloride and 36mg of terephthalic acid in DMF (18mL), dissolve it ultrasonically at room temperature, and then add 36mg of Fe 3 O 4 SiO 2 Then it was sealed in a 25mL hydrothermal reactor, and the reaction mixture was heated to 135°C, maintained at this temperature for 24 hours, and then cooled to room temperature. After the post-treatment, the target product can be obtained by circulating 4 times.

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Abstract

The invention discloses a preparation method and application of Fe3O4@SiO2@Zr-MOF. A synthesizing method of the magnetic hybrid MOF includes: under a hydrothermal condition, sealing Fe3O4@SiO2 particles and mixed solution, dissolved into DMF, of zirconium chloride and terephthalic acid into a 25ml reaction kettle, heating to certain temperature, keeping the temperature for 24 hours, cooling to room temperature, performing certain post-treatment, and circulating for three times to obtain the Fe3O4@SiO2@Zr-MOF. The Fe3O4@SiO2@Zr-MOF prepared by the method is good in magnetic response, good in stability, thick and adjustable in MOF layer, and the like, good absorption material can be obtained, and the Fe3O4@SiO2@Zr-MOF has application potential in organic dye absorption.

Description

Technical field [0001] The invention belongs to the technical field of water treatment, and specifically relates to a Fe 3 O 4 SiO 2 The preparation method of Zr-MOF and its application to the adsorption of 2-nitro-1,3-benzenediol. Background technique [0002] MOF material is a metal-organic framework material developed in recent decades and can be used in the fields of gas adsorption, organic adsorption, heavy metal ion adsorption, catalysis, and drug release. In 2012, Huang Yuting and others studied the Zr-MOF type materials in CO 2 Adsorption and CO 2 / N 2 Selective adsorption. In 2014, He Qinqin and others studied PANI / N-K 2 Ti 4 O 9 / Zr-MOF photocatalytic performance, Gregory W. Peterson studied the ability of Zr-MOF-NH2 to remove poisonous gas. HeQinqin studied the adsorption performance of Zr-MOF on the dye rhodamine B. Zr-MOF has applications in gas adsorption, catalysis and other fields, but it is very rare to apply to the adsorption of organic molecules after being c...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F101/38C02F101/34
CPCB01J20/223B01J20/0229B01J20/103B01J20/28009C02F1/288C02F2101/34C02F2101/38
Inventor 杨清香陈志军方少明赵倩倩蒋玲
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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