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Bifunctional group MOFs material and preparation method and application thereof

A bifunctional group, tertiary amine group technology, applied in chemical instruments and methods, other chemical processes, alkali metal oxides/hydroxides, etc., can solve the structural damage of ZIF-8 adsorbent, heavy metal cations and harmful Anion removal and regeneration does not have problems such as evaluation research and stability degradation, so as to improve the efficiency and success rate of synthesis and preparation, solve the secondary pollution of regenerant, and the preparation process is simple and easy to operate.

Active Publication Date: 2019-04-12
NANJING UNIV
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AI Technical Summary

Problems solved by technology

Although MOFs have good adsorption properties, desorption regeneration is still a challenging problem.
Li et al. (J.Phys.Chem.C., 2014) regenerated the As(V)-adsorbed ZIF-8 material through a higher concentration of HNO3 and HCl, which can make the regeneration rate of ZIF-8 reach 90% The above, but due to the use of strong acid regeneration, the structure of ZIF-8 adsorbent will be damaged to a certain extent, the stability will decrease, and the continuous regeneration performance will be poor. After three times of acid treatment, the regeneration rate will drop to about 80%. At the same time, this acidic regeneration The liquid will cause secondary pollution problems, which is not conducive to environmental protection; Daniel T.Sun et al. (ACSCent.Sci., 2018) used complexing agents such as ascorbic acid to study Fe-BTC materials that adsorb Pb(II) and Hg(II) Regeneration, this method effectively regenerates the adsorbent by complexing Pb(II) and Hg(II), and the regeneration rate can reach more than 95%. This method does not destroy the structure of the Fe-BTC adsorbent, so it can be regenerated after 10 cycles The efficiency remains above 90%, but this method requires a large amount of complexing agent, which causes energy consumption, and it is still a problem to deal with the complexing agent after regeneration
Existing reports have shown that RanwenOu et al. (Adv. Mater., 2018) achieved desalination and effective regeneration of MOFs through temperature control, but there is no evaluation study on the removal and regeneration of heavy metal cations and harmful anions

Method used

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  • Bifunctional group MOFs material and preparation method and application thereof
  • Bifunctional group MOFs material and preparation method and application thereof
  • Bifunctional group MOFs material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] First, the preparation method of carboxyl-functionalized ZIF-8 (ZIF-8-COOH) is as follows: Weigh 2.933 g of zinc nitrate hexahydrate and 6.489 g of 2-methyl-1H-imidazole-4,5-dicarboxylic acid, Then add 200ml of methanol solution and stir vigorously for 2h, then centrifuge and wash 3 times with methanol and deionized water respectively, then vacuum dry at 40°C for 24h to obtain a white powder of ZIF-8-COOH functionalized in situ with carboxyl group (such as figure 1 shown), with carboxyl functional groups.

[0045] The preparation steps of the bifunctional group MOFs material in this example are as follows:

[0046] Step 1: Grind the ZIF-8-COOH material. After the grinding is completed, add 0.5g of ZIF-8-COOH and 0.25g of DMAEA into 10ml of ethanol solution and stir evenly (the mass of ZIF-8-COOH and DMAEA The ratio is 2:1), then slowly add 0.01g of AIBN (the amount of AIBN accounts for 1.3% of the total mass fraction of MOFs and DMAEA), stir at 50°C for 12h, and obtain...

Embodiment 2

[0057] The preparation steps of ZIF-8-COOH in this example are the same as those in Example 1.

[0058] In this embodiment, the bifunctional group MOFs material (ZIF-8-COOH / R 2 N) The preparation steps are as follows:

[0059] Step 1: Grind the ZIF-8-COOH material. After the grinding is completed, add 0.5g ZIF-8-COOH and 1gDMVBA to 20ml of ethanol solution and stir evenly (the mass ratio of ZIF-8-COOH to DMVBA is 2: 4), then slowly add 0.15g AIBN (the amount of AIBN accounts for 10% of the total mass fraction of MOFs and DMVBA), stir at 55°C for 12h, and obtain precursor A after the ethanol is completely volatilized;

[0060] Step 2: Put the precursor A in an oven at 65°C for 12 hours to dry, and obtain the modified bifunctional group MOFs material after heating.

[0061] The bifunctional group MOFs material prepared in this example (ZIF-8-COOH / R 2 N), the specific surface area is 800m 2 / g; mesopore average pore diameter is 0.95nm; pore volume is 0.45cm 3 / g; the molar r...

Embodiment 3

[0068] The preparation steps of ZIF-8-COOH in this example are the same as those in Example 1.

[0069] In this embodiment, the bifunctional group MOFs material (ZIF-8-COOH / R 2 N) The preparation steps are as follows:

[0070] Step 1: Grind the ZIF-8-COOH material. After the grinding is completed, add 0.5g of ZIF-8-COOH and 0.5g of DMAEA into 15ml of ethanol solution and stir evenly (the mass of ZIF-8-COOH and DMAEA The ratio is 1:1), then slowly add 0.05g of AIBN (the amount of AIBN accounts for 5% of the total mass fraction of MOFs and DMAEA), stir at 70°C for 12h, and obtain the precursor A after the ethanol is completely volatilized;

[0071] Step 2: Put the precursor A in an oven at 70°C to dry for 6 hours, and obtain the modified bifunctional group MOFs material (ZIF-8-COOH / R 2 N).

[0072] The bifunctional group MOFs material prepared in this example (ZIF-8-COOH / R 2 N), the specific surface area is 900m 2 / g; mesopore average pore diameter is 1.05nm; pore volume is...

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Abstract

The invention discloses a bifunctional group MOFs material and a preparation method and application thereof, and belongs to the field of sewage treatment of nanometer composite functional materials. For the problems that existing MOFs materials cannot simultaneously remove anion and cation pollutants in water, the regeneration rate after adsorption is low, the regeneration effect is not ideal, andsecondary pollution is easily caused in the regeneration process, the bifunctional group MOFs has a carboxylic acid functional group and a tertiary amine group at the same time and can simultaneouslyremove anions and cations in the water; after adsorption is completed, the material is treated at a certain temperature, and the purposes of environmental protection and regeneration can be achieved.The preparation method is simple in process, easy to operate, environmentally friendly and free of pollution.

Description

technical field [0001] The invention belongs to the field of sewage treatment of nanocomposite functional materials, and more specifically relates to a dual-functional group MOFs material and its preparation method and application. Background technique [0002] Heavy metal cations are generally known to be highly bioaccumulative, highly toxic, and difficult to biodegrade, but at the same time, harmful anions in drinking water are another major pollutant in addition to metal cations. Anions in water Excessive pollutants will cause serious environmental and human health problems, so the removal of anionic pollutants in water is also very important. The secondary effluent from electroplating, mining and metallurgy industries after physical and chemical pretreatment and biochemical treatment contains not only heavy metal cations but also a variety of harmful anion pollutants (ClO 4 - , SO 4 2- , NO 3 - , F - etc.), the test results show that the residual concentration of ...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/22B01J20/28B01J20/30C02F1/28
CPCB01J20/226C02F1/288C08G83/008B01J20/28064B01J20/28071B01J20/28073B01J20/2808B01J20/3078B01J20/3085
Inventor 张炜铭计成汉李婷潘丙才花铭吕路
Owner NANJING UNIV
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