Hydrophobic graphdiyne composite iron-containing MOF adsorbent and preparation method thereof

A graphdiyne and adsorbent technology is applied in the field of preparation of highly hydrophobic graphdiyne composite adsorbents, which can solve the problems of MOFs skeleton collapse, reduce MOFs adsorption of VOCs, etc. The effect of water performance

Active Publication Date: 2020-07-10
GUANGXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The higher the concentration of water vapor, the more water molecules will be adsorbed into the pores of MOFs, thereby reducing the ability of MOFs to adsorb VOCs.
In addition, after too many water molecules coordinate with the metal, it is possible to dissociate the coordination bond between the metal and the ligand in the MOFs secondary unit structure through competitive coordination, resulting in the collapse of the MOFs skeleton.

Method used

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  • Hydrophobic graphdiyne composite iron-containing MOF adsorbent and preparation method thereof
  • Hydrophobic graphdiyne composite iron-containing MOF adsorbent and preparation method thereof
  • Hydrophobic graphdiyne composite iron-containing MOF adsorbent and preparation method thereof

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Effect test

Embodiment 1

[0039] A preparation method of a hydrophobic graphyne composite iron-containing MOF adsorbent, comprising the steps of,

[0040] (1) Preparation of MOF(Fe) seed crystals: first, ultrasonically disperse 1.0mmoL trimesic acid and 1.0mmoL ferric nitrate nonahydrate in an aqueous solution, and then place them in a stirrer to stir, (ferric nitrate nonahydrate and trimesis The molar ratio of acid is (1:1)). The solution was then put into a high-pressure reactor and placed in a programmed oven, and the temperature was raised to 150° C. at a rate of 10° C. / min for another 24 hours. The obtained MOF(Fe) material is ground to a particle size of <1.0 μm. Recorded as MOF(Fe) seed crystal.

[0041] (2) Preparation of MOF(Fe) seed crystal Pickering emulsion: first, place the ground MOF(Fe) seed crystal in the aqueous solution to obtain solution A: the input quality of the MOF(Fe) seed crystal is 2 mg, and the aqueous solution The total volume is 20mL; configure copper acetate aqueous sol...

Embodiment 2

[0045] A preparation method of a hydrophobic graphyne composite iron-containing MOF adsorbent, comprising the steps of,

[0046] (1) Preparation of MOF(Fe) seed crystals: first, ultrasonically disperse 1.0mmoL trimesic acid and 1.78mmoL ferric nitrate nonahydrate in aqueous solution, and then place them in a stirrer to stir, (ferric nitrate nonahydrate and tribenzene The molar ratio of the triacids is 1:1.78). The solution was then put into a high-pressure reactor and placed in a programmed oven, and the temperature was raised to 150° C. at a rate of 2° C. / min for another 24 hours. The obtained MOF(Fe) material is ground to a particle size of <1.0 μm. Recorded as MOF(Fe) seed crystal.

[0047] (2) Preparation of MOF(Fe) seed crystal Pickering emulsion: first, place the ground MOF(Fe) seed crystal in the aqueous solution to obtain solution A: the input quality of the MOF(Fe) seed crystal is 100mg, and the aqueous solution The total volume is 100mL; configure copper acetate a...

Embodiment 3

[0051] A preparation method of a hydrophobic graphyne composite iron-containing MOF adsorbent, comprising the steps of,

[0052] (1) Preparation of MOF(Fe) seed crystals: First, 1.0mmoL trimesic acid and 1.6mmoL ferric nitrate nonahydrate were ultrasonically dispersed in an aqueous solution (the molar ratio of ferric nitrate nonahydrate to trimesic acid was 1:1.6) , and then stirred in a blender. Then put the solution into a high-pressure reactor and place it in a programmed oven, and raise the temperature to 100° C. at a rate of 2° C. / min and keep the reaction for 20 hours. The obtained MOF(Fe) material is ground to a particle size of <1.0 μm. Recorded as MOF(Fe) seed crystal.

[0053] (2) Preparation of MOF(Fe) seed crystal Pickering emulsion: first put the ground MOF(Fe) seed crystal into the aqueous solution to obtain solution A: the input quality of the MOF(Fe) seed crystal is 70mg, and the aqueous solution The total volume is 80mL; configure copper acetate aqueous sol...

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Abstract

The invention discloses a hydrophobic graphdiyne composite iron-containing MOF adsorbent and a preparation method thereof. The method comprises the following steps: firstly, grinding MOF (Fe) into small-particle seed crystals, and dispersing the small-particle seed crystals into a copper acetate aqueous solution by using ultrasonic waves; adding dichloromethane into the solution, and stirring at ahigh speed to prepare a Pickering emulsion; dissolving hexacetenyl benzene into a certain amount of dichloromethane, and adding the mixture into the Pickering emulsion; growing graphdiyne on an emulsion interface containing a Cu catalytic site, then heating in a water bath to remove an organic phase, and centrifugally separating out graphdiyne composite seed crystals MOF (Fe); and finally, putting the graphdiyne composite seed crystals MOF (Fe) into ferric nitrate nonahydrate and trimesic acid to carry out secondary hydrothermal growth of MOF (Fe) crystals to obtain the high-hydrophobicity graphdiyne composite MOF (Fe) adsorbent. The stability of the Pickering emulsion is controlled by controlling the addition amount of MOF (Fe) and the ratio of a water phase to an oil phase, so that theaction between graphdiyne and MOF (Fe) seed crystals is influenced, the growth of MOF (Fe) is influenced, and the final hydrophobicity of the adsorbent and the preferential selective adsorption on hydrocarbon VOCs are effectively improved.

Description

technical field [0001] The invention belongs to the field of novel functional materials, and in particular relates to the preparation of a highly hydrophobic graphyne composite adsorbent. Background technique [0002] Metal-organic framework materials (MOFs) have become a new type of porous adsorption material that has attracted the most attention at home and abroad in the past two decades due to their huge specific surface area and adjustable pore structure, and have continuously refreshed the adsorption capacity of several typical VOCs. highest record. Relevant research reports show that MOFs materials will have great development potential and application prospects in the field of VOCs pollution control in the future. However, in recent years, researchers have found that in many laboratories, MOFs materials with strong adsorption capacity for VOCs, once they encounter a high-humidity environment (relative humidity greater than 50%), their adsorption capacity will drop sha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30B01J20/22B01J20/28B01D53/02
CPCB01J20/226B01J20/20B01J20/28014B01D53/02B01D2257/708B01D2257/702B01D2253/102B01D2253/204Y02A50/20
Inventor 赵祯霞张正生王睿猛赵钟兴
Owner GUANGXI UNIV
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