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A method for rapid preparation of amide-type octahedral MOFs at room temperature using copper formate as a raw material
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A technology of octahedron and copper formate, which is applied in the field of preparing micro-sized MOFs crystals, can solve the problems of small reaction capacity, unfavorable promotion and use, and high cost, and achieve the effect of reducing reaction time and being suitable for large-scale promotion and use
Active Publication Date: 2021-03-16
XIAN TECH UNIV
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[0003] At present, in the preparation of metal-organic frameworks (MOFs), the main method is to use a hydrothermal reactor at 70-80 ° C for 2-4 days. However, the reaction capacity of this method is small and the cost is high, which is not conducive to large-scale promotion and use.
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Embodiment 1
[0049] Under normal temperature and magnetic stirring conditions, pour the ligand N,N′,N″-tri-(3,5-dicarboxy 5mL DMF (0.0017mol / L) solution of phenyl)-1,3,5-tris-carbamoylbenzene 5.8mg, the solution slowly appeared blue precipitate, centrifuged, DMF washed three times, absolute ethanol washed three times, and Stored in absolute ethanol, the sample is characterized as figure 1 a, figure 2 as shown in a.
Embodiment 2
[0051] Under normal temperature and magnetic stirring conditions, pour the ligand N,N′,N″-tri-(3,5-dicarboxy 5mL DMF (0.0033mol / L) solution of phenyl)-1,3,5-tris-carbamoylbenzene 11.6mg, the solution slowly appears blue precipitate.Centrifugal separation, DMF washes three times, absolute ethanol washes three times, and Stored in absolute ethanol, the samples were characterized as figure 1 b, figure 2 as shown in b.
Embodiment 3
[0053] Under normal temperature and magnetic stirring conditions, pour the ligand N,N' dissolved in 5mL DMF (N,N'-dimethylformamide) (0.015mol / L) solution dissolved with 16.9mg copper formate tetrahydrate, N″-tris-(3,5-dicarboxyphenyl)-1,3,5-tris-carbamoylbenzene 17.5mg in 5mL DMF (0.005mol / L) solution, the solution slowly appeared blue precipitate, centrifuged , washed three times with DMF, washed three times with absolute ethanol, and stored in absolute ethanol, the sample characterization is as follows figure 1 c, figure 2 as shown in c.
[0054] Depend on figure 1 It can be seen that the crystal morphology of the products prepared in the above-mentioned Examples 1 to 3 is octahedral, and the size is 1.5-10 μm. Depend on figure 2 As can be seen, the products obtained in the above-mentioned embodiment one to embodiment three, figure 2 a. figure 2 b and figure 2 The baseline in c is flat, there are few interference peaks, and the highest peak is relatively strong,...
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Abstract
The invention discloses a method for rapidly preparing amide type octahedral metal-organic frameworks (MOFs) at the room temperature by using copper formate as a raw material. The method comprises thefollowing steps: dissolving copper formate tetrahydrate into a dimethyl formamide (DMF) solvent to prepare a salt solution, wherein the concentration of the copper formate tetrahydrate in the salt solution is 0.003-0.015mol / L; dissolving N, N', N''-tris-(3, 5-dicarboxyphenyl)-1, 3, 5-tri-carbamyl benzene into the DMF solvent to obtain a ligand solution, wherein the concentration of the N, N', N''-tris-(3, 5-dicarboxyphenyl)-1, 3, 5-tri-carbamyl benzene in the ligand solution is 0.0017-0.005mol / L; adding the ligand solution into the salt solution, wherein the volume of the added ligand solution is equal to that of the salt solution, and standing for carrying out a reaction until blue precipitate is generated in the solution so as to obtain a solution containing the amide type octahedral MOFs material; centrifuging the solution containing the amide type octahedral MOFs material, and washing to obtain the amide type octahedral MOFs material. The method provided by the invention is used for preparation at the room temperature, shortens the preparation reaction time, and increases the production efficiency.
Description
【Technical field】 [0001] The invention belongs to the technical field of preparing micro-sized MOFs crystals, in particular to a method for rapidly preparing amide-type octahedral MOFs at room temperature using copper formate as a raw material. 【Background technique】 [0002] In recent years, metal-organic frameworks (MOFs) have broad application prospects in energy and environment fields such as gas storage, gas separation, and photochemical sensors due to their large specific surface area, variable structure, and adjustable functions. [0003] At present, in the preparation of metal-organic frameworks (MOFs), the main method is to use a hydrothermal reactor at 70-80 ° C for 2-4 days. However, the reaction capacity of this method is small and the cost is high, which is not conducive to large-scale promotion and use. . 【Content of invention】 [0004] The purpose of the present invention is to provide a method for rapidly preparing amide-type octahedral MOFs at room temper...
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