A ferrous-based metal-organic framework material, its atmospheric pressure synthesis method, and a method for catalytically activating persulfate to treat organic pollutants

A technology of organic pollutants and organic frameworks, applied in organic compound/hydride/coordination complex catalysts, water pollutants, oxidized water/sewage treatment, etc., can solve the problem of unstable activation effect, harsh synthesis conditions, pH value It can achieve the effect of broad practical application prospects, low requirements for synthesis equipment and good durability.

Active Publication Date: 2022-03-29
广东顺控自华科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of harsh synthesis conditions of metal organic framework materials, low activation efficiency of traditional catalysts in the activated PS system, great influence of pH value, easy to cause secondary pollution, unstable activation effect of existing metal organic framework materials, etc. , successfully achieved good results in the experiment of activating persulfate to degrade POPs pollutants under a wide range of pH conditions using a heterogeneous catalyst synthesized at atmospheric pressure with a high proportion of ferrous-based metal-organic framework materials (Fe(II)-MOFs). solution effect

Method used

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  • A ferrous-based metal-organic framework material, its atmospheric pressure synthesis method, and a method for catalytically activating persulfate to treat organic pollutants
  • A ferrous-based metal-organic framework material, its atmospheric pressure synthesis method, and a method for catalytically activating persulfate to treat organic pollutants
  • A ferrous-based metal-organic framework material, its atmospheric pressure synthesis method, and a method for catalytically activating persulfate to treat organic pollutants

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In this example, the effects of different pH values ​​on the catalytic activation of PS to degrade DBP by Fe(II)-MOFs were compared.

[0039] (1) Preparation of Fe(Ⅱ)-MOFs: Take terephthalic acid (1.065g) and FeCl respectively 2 4H 2 O (2.65g) was placed in a 500ml three-necked flask, and 250ml of N,N-dimethylformamide was added to dissolve it, then 30ml of methanol was added, and 8ml of hydrofluoric acid was added dropwise to make the solution light green, and then dried with The nitrogen gas removes dissolved oxygen from the mixture. The synthesis conditions were controlled to the following five types: 140°C&24h, 140°C&18h, 140°C&12h, 120°C&24h and 100°C&24h, respectively named as Fe(Ⅱ)-MOFs-1 / 2 / 3 / 4 / 5, in Cool to room temperature under a dry nitrogen atmosphere. After the three-necked flask is cooled, transfer the reacted mixture to a centrifuge tube, and centrifuge at 10,000rpm for 10 minutes to separate the solid; then pour the solid into a beaker, wash with meth...

Embodiment 2

[0047] In this example, the effects of different pH values ​​on the catalytic activation of PS to degrade DBP by Fe(II)-MOFs were compared.

[0048] (1) Preparation of Fe(Ⅱ)-MOFs: Take terephthalic acid (1.065g) and FeCl respectively 2 4H 2 O (2.65g) was placed in a 500ml three-necked flask, and 250ml of N,N-dimethylformamide was added to dissolve it, then 30ml of methanol was added, and 8ml of hydrofluoric acid was added dropwise to make the solution light green, and then dried with The nitrogen gas removes dissolved oxygen from the mixture. The mixture was heated to 140° C., stirred under a dry nitrogen atmosphere for 24 h, then stopped heating, and cooled to room temperature under a dry nitrogen atmosphere. After the three-necked flask is cooled, transfer the reacted mixture to a centrifuge tube, and centrifuge at 10,000rpm for 10 minutes to separate the solid; then pour the solid into a beaker, wash with methanol for 1 hour, and centrifuge for 3 times. Put them into a v...

Embodiment 3

[0056] The present embodiment compares the different mol ratios of PS and DBP (n Na 2 S 2 o 8 / n DBP=30, 50, 150, 200, 250, 300, 350) on the catalytic activation of Fe(Ⅱ)-MOFs.

[0057] (1) The preparation method of Fe(II)-MOFs is the same as step (1) in Example 2;

[0058] (2) The DBP solution of 0.018mmol / L is standby;

[0059] (3) Using conical flask as reactor, add 0.054, 0.090, 0.180, 0.270, 0.360, 0.450, 0.540mmol Na in the reactor 2 S 2 o 8 and 0.018mmol / L DBP 100mL, add 0.03g metal organic framework material to the reactor at the same time, place the Erlenmeyer flask in a shaker at 180rpm, react at normal temperature (25°C), and take samples for analysis at fixed points;

[0060] (4) Add 0.090mmol Na to the reactor 2 S 2 o 8 , other conditions are the same as (3);

[0061] (5) Add 0.180mmol Na to the reactor 2 S 2 o 8 , other conditions are the same as (3);

[0062] (6) Add 0.270mmol Na to the reactor 2 S 2 o 8 , other conditions are the same as (3); ...

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Abstract

The invention discloses a ferrous-based metal-organic framework material, a normal-pressure synthesis method thereof, and a method for treating organic pollutants by catalytically activating persulfate. This method successfully synthesized heterogeneous catalysts with a high proportion of ferrous-based metal-organic frameworks (Fe(II)-MOFs) under normal pressure. Taking advantage of the characteristics of high active sites and strong catalytic activity of metal-organic frameworks, it catalyzes Activated persulfate generates sulfate radicals to degrade persistent organic pollutants. The catalyst is easy to recycle and use, and the activation effect is still good after repeated use, and is an environment-friendly material. The method is suitable for a variety of persistent organic pollutants, has good persistence, short catalytic time, convenient operation, and has a high degradation effect in a wide range of pH values, and has great advantages in degrading persistent organic pollutants. Great application prospects.

Description

technical field [0001] The invention belongs to the technical field of water pollution control, and in particular relates to a ferrous-based metal-organic framework material, a normal-pressure synthesis method thereof, and a method for treating organic pollutants by catalytically activating persulfate. Background technique [0002] Based on sulfate radical (SO4 - ·) advanced oxidation technology, due to its high efficiency in degrading pollutants, has received more and more attention and attention from researchers in the field of degrading persistent organic pollutants. In existing reports, photoactivation, heat activation, ultrasound, and metal ion activation are generally used to generate sulfate radicals for PS. However, traditional catalytic activation methods have low efficiency, are greatly affected by pH, and easily cause secondary pollution. However, it is difficult to be widely used in practical industry. The use of metal-organic frameworks as heterogeneous cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/16B01J35/02C02F1/72C02F101/30
CPCC02F1/725B01J31/1691B01J35/02C02F2101/30
Inventor 万金泉池海远马邕文王艳
Owner 广东顺控自华科技有限公司
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