SYNTHESIS, STRUCTURE, AND CHEMICAL PROPERTIES OF MOF BASED ON 4 ACETAMIDOBENZOIC ACID AND Ag (I)

“TIBBIYOT OLIYGOHLARIDA TABIIY FANLARNI

INTERFAOL USULLARDA O'QITISHNING

MUAMMOLARI VA YECHIMLARI”

123

SYNTHESIS, STRUCTURE, AND CHEMICAL PROPERTIES OF MOF BASED ON 4-

ACETAMIDOBENZOIC ACID AND Ag (I)

1

Ibragimov A.B.,

1

Dusimbetova Sh.Y.,

1

Begjanova G.B

.,

2

Rasulova S.M.

1

Institute of General and Inorganic Chemistry, Academy of Sciences of Uzbekistan, Tashkent,

2

Termiz State University, Barkamol Avlod Street, Termiz

dusimbetovashaxnoza@gmail.com

Annotation.

The ligand 4-acetamidobenzoic acid and other ligand diphenylamine and its

complex compounds of and silver(nitrates) were synthesized. The composition and structure of the
synthesized compounds were studied by method of IR spectroscopy.

Keywords

: MOF, 4-acetamidobenzoic acid, diphenylamine, ligand, IR spectrum, synthesis

Introduction:

Metal-organic frameworks (MOFs) are crystalline porous materials composed of a coordinated

combination of metal ions or clusters and organic ligands, possessing a high surface area, adjustable
pore size, various functional groups, and high thermal stability. [1, 2]

They have a flexible structure and are widely used in electrochemical systems, gas storage,

separation, catalysis [2, 3], heavy metal removal, drug delivery, water purification, energy storage,
photocatalysis, sensors, biomedicine, and many other fields. Currently, more than 20,000 MOFs have
been synthesised, differing in design, structure, synthesis method, and degree of porosity. [2,4]

There are several methods for obtaining MOFs, including classical (including solvothermal),

microwave, electrochemical, mechanochemical, and ultrasonic methods. Typically, MOFs crystallise
in a solution medium. [4] In the synthesis of this MOF, we used the ultrasonic method and studied
the IR spectrum of this framework.

The selection of ligands also plays a crucial role in MOF synthesis. For this reason, we chose

4-acetamidobenzoic acid from among numerous ligands. Although there are studies on discrete
complexes based on 4-acetamidobenzoic acid, metal complexes of acetamidobenzoic acids with
mixed ligands, especially coordination polymers, have not yet been sufficiently investigated. [5]
Therefore, we studied the synthesis of MOF using this ligand in the presence of AgNO₃ and examined
its IR spectral properties.

Experimental.

In this study, MOF, structure, and physicochemical properties of the

synthesized polymer were determined using IR spectroscopy analysis.

Synthesis:

0.27 g (0.0015 mol) of 4-acetamidobenzoic acid was dissolved in 30 ml of DMF,

and 15 ml of a 0.05 mol·L−1 solution prepared from 0.127 g of AgNO3 was added to it. The mixture
was stirred at a constant speed in a magnetic stirrer for 30 minutes. The resulting black solution was
treated with an ultrasonic sonicator with a power of 500 W for 20 minutes, accelerating the formation
of the complex. The mixture was filtered, and the purified filtrate was stored in a thermostat at 50-
60°C for 25 days for crystallization. As a result, brown, diamond-shaped crystals were obtained. The
yield was 75%

(Figs. 1 and 2).

Fig. 1 MOF synthesis reaction

“TIBBIYOT OLIYGOHLARIDA TABIIY FANLARNI

INTERFAOL USULLARDA O'QITISHNING

MUAMMOLARI VA YECHIMLARI”

124

Fig. 2 MOF crystal production scheme

FT-IR analysis

. In the IRT spectrum of MOF synthesized on the basis of 4-acetamidobenzoic acid

and AgNO

3

, O-H and N-H stretching vibrations were observed at 3307 and 3043 cm

−1

, and amide

C=O stretching vibrations at 1670 cm

−1

. The peaks in the range of 1581-1418 cm

−1

belong to the

aromatic ring and COO

−

groups. C-N and C-O bonds are detected at 1305-869 cm

−1

. Peaks in the

range of 740-425 cm

−1

confirm Ag-O and Ag-N coordination bonds. This indicates the formation of

the MOF structure

(Figure 3).

Fig. 3 MOF spectrum of a polymer compound

References

1.Lalawmpuia R. et al. Metal organic framework (MOF): Synthesis and fabrication for the

application of electrochemical sensing //Environmental Engineering Research. – 2024. – Т. 29. – №.
5.

doi:10.20944/preprints202309.0192.v1

2.

Kaushal S. et al. First transition series metal–organic frameworks: Synthesis, properties

and applications //Materials Advances. – 2021. – Т. 2. – №. 22. – С. 7308-7335.

DOI:

10.1039/d1ma00719j

3.Wang W. et al. Two-dimensional metal-organic frameworks: from synthesis to

bioapplications //Journal of Nanobiotechnology. – 2022. – Т. 20. – №. 1. – С.
207.

https://doi.org/10.1186/s12951-022-01395-9

4.Butova V. V. et al. Metal-organic frameworks: structure, properties, methods of synthesis

and characterization //Russian Chemical Reviews. – 2016. – Т. 85. – №. 3. – С.
280.

DOI:

10.1070/RCR4554

5.Bai E. H. P., Vairam S. Spectral and thermal studies of transition metal complexes of

Acetamido Benzoic Acids with hydrazine //Asian Journal of Chemistry. – 2013. – 6.Т. 25. – №. 1. –
С. 209.

http://dx.doi.org/10.14233/ajchem.2013.12895

FujitaMKwonY JWashizuSOguraK 1994 J. Am. Chem. Soc. 116 1151

http://dx.doi.org/10

.

7.SeoJ SWhangDLeeHJunS IOhJJeonY JKimK 2000 Nature 404 982

http://dx.doi.org/10

.

8.HasegawaSHorikeSMatsudaRFurukawaSMochizukiKKinoshitaYKitagawaS 2007 J. Am.

Chem. Soc. 129 2607

http://dx.doi.org/10.1021/ja067374y

9.Gomez-LorBGutierrez-PueblaEIglesiasMMongeM ARuiz-ValeroCSnejkoN 2005 Chem.

Mater. 17 2568

http://dx.doi.org/10.1021/cm047748r