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Ti-based MOF composite material, and preparation method and application thereof

A composite material, diethylaniline technology, applied in chemical instruments and methods, catalyst activation/preparation, water treatment of special compounds, etc., can solve the problems of high energy consumption, damage to the original material structure, etc., to increase the number of photogenerated electrons, The preparation method is simple and safe, and the effect of good recovery and recycling

Active Publication Date: 2020-07-03
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Loading heavy metal nanoparticles on the surface of materials has been proved to be an effective means to improve the performance of materials, but the commonly used ultraviolet light reduction method and NaBH4 Reduction by other reducing agents has the disadvantages of high energy consumption or easy damage to the original material structure

Method used

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  • Ti-based MOF composite material, and preparation method and application thereof
  • Ti-based MOF composite material, and preparation method and application thereof
  • Ti-based MOF composite material, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] MR / NH 2 -The preparation method of MIL-125 composite material, comprising steps:

[0052] (1) Dissolve 3.85 g of 2-aminoterephthalic acid (ATA) and 4.2 mL of butyl titanate in 14 mL of anhydrous methanol and 56 mL of anhydrous N,N-dimethylformamide (DMF) in a round bottom flask Mix the solution, use a reflux condenser, heat and stir, keep the solution temperature at 100°C and reflux for 72h, cool to room temperature and filter the mixture, separate the solid, wash with DMF at 155°C for 24h, then wash with methanol at 100°C, the product Dry in air at 100 °C and triturate to give NH 2 - MIL-125(Ti) powder.

[0053] (2) 200mg NH 2 -MIL-125(Ti) suspended in 90mL water to form a suspension, 22.75mg NaNO 2 (330μmol, NH 2 -MIL-125(Ti) with NaNO 2 The molar ratio is 1:3) dissolved in the above MOF aqueous suspension. The temperature was cooled in an ice-water bath and kept at 0°C, and the stirring was continued. 60 mL of 0.03M HCl was added dropwise, and the stirring was...

Embodiment 2

[0058] Taking the reduction of chromium-containing Cr(VI) waste water as an example to test the single NH of embodiment 1 2 -MIL-125(Ti), MR / NH 2 The catalytic activity of -MIL-125 composite catalyst and single MR-MIL-125 (Ti), in the chromium-containing Cr (VI) wastewater that adding volume is 100mL, concentration is 80 μ mol / L in the reactor, adds 10mg above-mentioned catalyst, Add EDTA-2Na at a concentration of 2mmol / L as a hole-scavenging agent for synergistic reaction, adjust pH=2, continue to stir, stir in the dark for 30min to adsorption equilibrium, turn on the visible light source, and carry out photocatalytic reaction for 120min.

[0059] Such as figure 2 , the MR / NH prepared in this example 2 -MIL-125 composite photocatalyst is superior to single NH 2 - MIL-125(Ti) catalyst, single MR-MIL-125(Ti), has the best visible light reduction effect of Cr(VI).

Embodiment 3

[0061] According to the preparation method of Example 1 steps (1)~(3), different amounts of nitrite NaNO were added during the preparation process 2 , can change NH 2-The ratio of diazotization reaction of MIL-125(Ti) to form MR / NH with different diazotization ratios 2 - MIL-125 composite catalyst. Add 9.1, 18.2, 22.75, 27.3, 36.4 mg NaNO respectively in the synthesis step (2) of Example 1 2 , making NaNO 2 with NH 2 -Amino group on MIL-125 (Ti) (according to 1mol NH 2 The molar ratios of the amino groups on MIL-125 (Ti) are 6 mol) are 0.2:1, 0.4:1, 0.5:1, 0.6:1, and 0.8:1, respectively.

[0062] Such as image 3 , MR / NH with different diazotization ratios prepared in this example 2 -Add NaNO to MIL-125 composite catalyst 2 When the molar ratio to amino group is 0.5:1, it has the best effect of reducing Cr(VI) with visible light.

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Abstract

The invention discloses an MR / NH2-MIL-125 composite material, a preparation method thereof, and an application of the MR / NH2-MIL-125 composite material in the field of photocatalysis. The preparationmethod comprises the following steps: (1) adding 2-aminoterephthalic acid and butyl titanate into a DMF / methanol solution, preparing NH2-MIL-125 by using a heating reflux method, and carrying out centrifugation, washing, drying and grinding treatment to obtain NH2-MIL-125(Ti) powder; (2) dispersing the NH2-MIL-125(Ti) powder into deionized water, stirring and mixing uniformly, adding NaNO2, dissolving, performing ice-water bath treatment to obtain a turbid liquid, dropwise adding hydrochloric acid, and continuously stirring; and (3) dropwise adding an acetic acid solution of diethylaniline into the mixed solution obtained in step (2), and carrying out a complete stirring reaction so as to obtain the MR / NH2-MIL-125 composite material.

Description

technical field [0001] The invention relates to the technical field of visible light catalysis, in particular to a Ti-based MOF composite material and a preparation method and application thereof. Background technique [0002] In recent years, the global environment has been severely polluted by toxic heavy metals due to the excessive discharge of pollutants produced in various industrial, agricultural, and mining processes. Hexavalent chromium (Cr(VI)) is a common pollutant in surface and groundwater, and it is widely used in electroplating, leather tanning, printing and other industries. Cr(VI)-contaminated aquatic ecosystems and drinking water sources can cause severe diarrhea and even various cancers, seriously threatening the environment and human health. Even at relatively low concentrations, Cr(VI) can still cause great harm to humans due to its high toxicity, carcinogenicity, and bioaccumulation through the food chain. [0003] Cr(III) is environmentally friendly a...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/00B01J37/16B01J37/34C02F1/30C02F101/22
CPCB01J31/1691B01J31/2239B01J37/16B01J37/344C02F1/30C02F2101/22C02F2305/10B01J2531/46B01J2540/40B01J35/39Y02W10/37Y02E60/36
Inventor 王齐傅炀杰毛惠秀翁文斌简育玲朱建旭
Owner ZHEJIANG GONGSHANG UNIVERSITY
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