Modified carbon nitride/Fe-based MOF composite material and preparation method and application thereof

A composite material and carbon nitride technology, applied in the field of visible light catalysis, can solve the problems of poor photoresponsiveness, high band gap, and small specific surface area, and achieve the effects of convenient synthesis, easy recycling, and high photocatalytic activity

Active Publication Date: 2020-07-14
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, TiO, which has been studied more 2 There are still some shortcomings in semiconductor catalysts such as small specific surface area, high band gap, and poor photoresponse ability. It is urgent to develop new and efficient visible light catalysts.

Method used

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  • Modified carbon nitride/Fe-based MOF composite material and preparation method and application thereof
  • Modified carbon nitride/Fe-based MOF composite material and preparation method and application thereof
  • Modified carbon nitride/Fe-based MOF composite material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] NH containing different proportions of aminoterephthalic acid ligands 2-MIL-53(Fe)-X% preparation

[0027] 1) NH 2 -MIL-53(Fe)-100% (i.e. NH 2 - Preparation of MIL-53(Fe))

[0028] First, 2mmol FeCl 3 ·6H 2 O and 2mmol of aminoterephthalic acid were dissolved in 40mL of N,N-dimethylformamide, magnetically stirred for 60min, then transferred to a hydrothermal kettle, heated at 150°C for 15h, naturally cooled to room temperature, at a rate of 8000rpm, Centrifuge for 5min, then wash twice with DMF and methanol respectively, and finally dry in vacuum at 100°C for 12h to obtain the NH 2 -MIL-53(Fe)-100%.

[0029] 2) NH 2 - Preparation of MIL-53(Fe)-75%

[0030] First, 2mmol FeCl 3 ·6H 2 O, 1.5mmol aminoterephthalic acid and 0.5mmol terephthalic acid were dissolved in 40mL of N,N-dimethylformamide, stirred by magnetic force for 60min, then transferred to a hydrothermal kettle, heated at 150°C for 15h, and naturally Cool to room temperature, centrifuge at 8000rpm fo...

Embodiment 2

[0042] g-C 3 N 4 Preparation of -M dispersion liquid (stripping liquid)

[0043] 1) g-C 3 N 4 -M preparation

[0044] Weigh melamine and triaminopyrimidine and mix them uniformly in a molar ratio of 1:3, spread them on a quartz boat, heat them in a tube furnace under nitrogen atmosphere, and raise the temperature to 500 °C at a heating rate of 5 °C / min. ℃ for 120 min, and finally cooled to room temperature under nitrogen purging to obtain powdery g-C 3 N 4 -M, after being ground into powder, sonicated in pure DMSO for 120min to exfoliate g-C 3 N 4 -M particles, centrifuged five times with distilled water at 8000 rpm in a centrifuge, and then dried in a vacuum oven at 60°C for 12 hours and collected.

[0045] 2) g-C 3 N 4 -M dispersion preparation

[0046] Weigh the good g-C prepared in step 1) 3 N 4 -M particles 50 mg, added to DMF and ultrasonicated for half an hour to obtain g-C with a concentration of 1 mg / mL 3 N 4 -M dispersion.

Embodiment 3

[0048] Preparation of multiple composite catalysts

[0049] 1) g-C 3 N 4 -M / NH 2 - Preparation of MIL-53(Fe)-50%

[0050] First, 2mmol FeCl 3 ·6H 2 O, 1mmol of aminoterephthalic acid and 1mmol of terephthalic acid were dissolved in 40mL of N-N-dimethylformamide, and different volumes (0.5mL, 1.0mL, 1.5mL, 2mL) of g-C prepared in Example 2 were added 3 N 4 -M dispersion liquid, magnetically stirred for 60min, then transferred to a hydrothermal kettle, heated at 150°C for 15h, cooled to room temperature naturally, centrifuged at 8000rpm for 5min, then washed twice with DMF and methanol respectively, and finally washed at 100 Vacuum drying at ℃ for 12h to obtain g-C 3 N 4 -M g-C with different loading ratios 3 N 4 -M / NH 2 -MIL-53(Fe)-50%.

[0051] 2) Performance test of photocatalytic reduction of Cr(VI)

[0052] Take 10mg g-C 3 N 4 -M g-C with different loading ratios 3 N 4 -M / NH 2 -MIL-53(Fe)-50%, added to the potassium dichromate solution (100mL) with a Cr(VI...

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Abstract

The invention discloses a modified carbon nitride/Fe-based MOF composite material and a preparation method and application thereof in the field of photocatalysis. The preparation method comprises thefollowing steps: (1) uniformly mixing melamine and triaminopyrimidine according to a molar ratio of 1:(2-4), performing roasting at 450-550 DEG C in an inert atmosphere, grinding the obtained product,adding the ground product into dimethyl sulfoxide, performing ultrasonic stripping for 1-3 hours, performing centrifuging with distilled water, performing washing and drying to obtain modified carbonnitride powder; and (2) dispersing the modified carbon nitride powder obtained in the step (1) into N, N-dimethylformamide; dissolving carbon nitride in N, N-dimethylformamide to form dispersion liquid, adding the dispersion liquid into an N, N-dimethylformamide solution containing ferric chloride, terephthalic acid and aminoterephthalic acid to uniformly mixing, and carrying out solvothermal reaction at 140-160 DEG C for 14-16 hours to obtain the modified carbon nitride/Fe-based MOF composite material.

Description

technical field [0001] The invention relates to the technical field of visible light catalysis, in particular to a modified carbon nitride / Fe-based MOF composite material and its preparation method and application. Background technique [0002] Taking the heavy metal chromium as an example, industries such as tanning and electroplating produce a large amount of chromium-containing Cr(VI) organic wastewater every year, and the resulting complex pollution is difficult to control and the toxicity is enhanced. So how to effectively remove Cr(VI) in water is an urgent problem to be solved. [0003] The traditional chemical reduction method requires step-by-step treatment and produces a large amount of chromium-containing sludge. Photocatalysis, as a clean and environment-friendly technology, can process Cr(VI)-containing complexes in one step due to its ability to generate electron-hole pairs under light and has redox properties. However, TiO, which has been studied more 2 Suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J37/08C02F1/72C02F1/30C02F101/22
CPCB01J31/1691B01J31/2239B01J35/004B01J37/08B01J37/084C02F1/725C02F1/30C02F2101/22C02F2305/10
Inventor 张柯杰胡晓张延硕郭佳允王齐
Owner ZHEJIANG GONGSHANG UNIVERSITY
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