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№ 1 (127)_химия и биология_январь. 2025 г.
SYNTHESIS AND ANALYSIS OF THE COORDINATION COMPOUND OF COPPER(II) M-HYDROXYBENZOATE WITH SODIUM GLYCINATE
Rakhila Kurbanova
PhD student, Khorezm Mamun Academy, Uzbekistan, Khiva
Shodlik Khasanov
Senior researcher, Khorezm Mamun Academy, Uzbekistan, Khiva
Zubayda Abdullaeva
Associate Professor, Urgench RANCH University of Technology, Uzbekistan, Urgench E-mail: [email protected]
СИНТЕЗ И АНАЛИЗ КООРДИНАЦИОННОГО СОЕДИНЕНИЯ М-ГИДРОКСИБЕНЗОАТА
МЕДИ(Н) С ГЛИЦИНАТОМ НАТРИЯ
Курбанова Рахила Салиевна
PhD докторант Хорезмской академии Мамуна, Узбекистан, г. Хива
Хасанов Шодлик Бекпулатович
Старший научний сотрудник, Хорезмская академия Маъмуна, Узбекистан, г. Хива
Абдуллаева Зубайда Шавкатовна
Доцент,
Ургенчский технологический университет RANCH,
Узбекистан, г. Ургенч E-mail: zubayda. abdullayeva.91@mail. ru
ABSTRACT
Optimum methods of synthesis of copper(II) m-hydroxybenzoate complex compound with sodium glycinate were studied based on literature analysis and synthesis was carried out. The factors affecting the synthesis of the resulting complex compound in room conditions were shown. In particular, the influence of temperature and the dependence of the reaction on time and concentration were studied in practice. The structure of the synthesized complex compound, the coordination bonds formed in it were studied using the method of infrared spectroscopy, the thermal stability was studied using the method of differential scanning colorometry, and its quantitative composition was studied using the methods of elemental analysis, and its chemical structure was determined, as well as this new complex compound proved to be thermally and chemically stable.
АННОТАЦИЯ
На основе анализа литературы изучены оптимальные методы синтеза комплексного соединения м-гидроксибензоата меди(П) с глицинатом натрия и проведен синтез. Показаны факторы, влияющие на синтез полученного комплексного соединения в комнатных условиях. В частности, на практике изучалось влияние температуры и зависимость реакции от времени и концентрации. Строение синтезированного комплексного соединения, образующиеся в нем координационные связи изучены методом инфракрасной спектроскопии, термостабильность - методом дифференциальной сканирующей колорометрии, его количественный состав -методами элементного анализа, была определена его химическая структура, а также это новое комплексное соединение оказалось термически и химически стабильным.
Библиографическое описание: Kurbanova R., Khasanov S., Abdullaeva Z. SYNTHESIS AND ANALYSIS OF THE COORDINATION COMPOUND OF COPPER(II) m-HYDROXYBENZOATE WITH SODIUM GLYCINATE // Universum: химия и биология : электрон. научн. журн. 2024. 1(127). URL: https://7universum.com/ru/nature/ar-chive/item/19067
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Keywords: Cu(II) m- hydroxobenzoate, complex compound, metal complex, elemental analysis, infrared (IR) spectroscopy, thermal analysis
Ключевые слова: Cu(II) м-гидроксобензоат, комплексное соединение, металлокомплекс, элементный анализ, инфракрасная (ИК) спектроскопия, термический анализ
Introduction. The study of coordination compounds allows us to explain their basic chemical properties, to form complexes, to determine the nature of chemical bonds between ligands, to use modern physical research to determine the mechanisms of processes involving coordination compounds and changes in the reactivity of coordinated ligands. The information obtained is important for the targeted discovery and synthesis of new chemical substances with a predetermined specific property, composition, structure, and other important properties [1]. This is especially necessary for substances with biologically active properties used in medicine [2]. Enzymes that function in the human body are also complex compounds by their chemical nature [3]. When poisoning with metals , they are treated by converting them into complex compounds and removing them from the body [4].
Experiments on obtaining oxide thin layers from Fe (III) salicylate were carried out. It is known that oxide layers serve as the main material for microelectronics and solar energy harvesting [5]. In this regard, it is known that Fe2O3 formed in the layer is suitable as a raw material for obtaining photoelectrochemical materials in solar energy conversion, as microelectronic conductors as a capacitor, and as a negative electrode in rechargeable batteries [6]. The scientific team proposed a method of forming a thin layer of Fe2O3 from iron salicylate salt in an ethanol medium. A dark red [FeC6H4OCOO]+ complex was formed from FeCl3 and salicylic acid added to an ethanol solution, in which the salicylate ligand binds bidentately to the Fe3+ ion through its O-phenolate and O-carboxylate oxygens. The reddening of the FeCl3-C6H4OHCOOH mixture in ethanol at a temperature of 60°C produced a solid layer and liquid dispersed form of iron (III) chloride salicylate salt in the ratio of 1:1. The composition of the solid layer corresponded to [FeC6H4OCOO]ClH2O and was stable up to 100°C. Oxidation of salicylate occurs only in the range of 210-600°C, and at the end it was observed that Fe2O3 hematite saltation appears from the complex. During experiments, the formation of iron salicylate complex was proved by UV-spectroscopy, thermal analysis [7].
A complex combination of uranium (IV) oxide was obtained in the presence of M-hydroxybenzoic acid [8]. When the single crystal of the complex was studied using an X-ray diffractometer, the coordination polygon of the uranium atom formed the shape of a hexagonal bipyramid through the O atoms of the carboxyl groups of 3 m-hydroxybenzoic acids.
One of the first works in the field of chemistry of polynuclear NYeE complexes was the study of octahedral hydroxonitrates [Ln6(|i6-0)(|i3-
Cu(C6I I4(OI I)COO)2 + 2NH2Ci I2COONa ■
H)8(NO3)6(H2O)x](NO3)2(Ln =Pr - Lu, x = 3 - 6 ), synthesized by careful heating and hydrolysis of the corresponding nitrates under the influence of an aqueous solution of alkali [9], then hydroxoperchlorates [Ln6(^6-OX^3-OHMH2O)24](ClO4)8 (Ln = Nd, Gd) [10] and hydroxoiodides [Ln6(^6-OX^3-OH)8(H2O)24]I8 (Ln = Nd, Eu, Tb, Dy) [11] were synthesized by the same method. A distinctive feature of these structures is the absence of organic ligands that could coordinate with metal ions to stabilize the polynuclear complex. This leads to the complexes being less stable in solution, both to deeper hydrolysis and to heating.
A more effective approach for the synthesis of stable polynuclear complexes was proposed by Zheng Zhiping. It consists in the partial hydrolysis of lanthanide compounds in aqueous solutions of amino acids, leading to the assembly of polynuclear complexes with the nucleus {Ln^-OH^}. The solutions of amino acids have buffer properties, which allows maintaining the pH during the synthesis process; this approach is called ligand-controlled hydrolysis. The polynuclear complexes described in the literature were synthesized using this approach.
Research Methodology. "Analytical grade" powders of CuCO3-Cu(OH)2, NaOH, m-hydroxybenzoic acid and glycines were used in the synthesis of the starting substances. The synthesis of the initial substances was carried out using the following methods: an alkali solution prepared in a 1:1 mol ratio was added to the glycine solution.
NH2CH2COOH + 2NaOH = NH2CH2COONa + H2O
To form a solution of copper (II) m-hydroxybenzoate, a solution of m-hydroxybenzoic acid measured in a ratio of 1:4 mol over malachite was added in an ultrasonic apparatus at a temperature of 550C and the reaction was carried out.
CuCO3 • Cu(OH)2 + 4HO-C6H4COOH = 2(HO-C6H4COO)2Cu + CO2Î + H2O
The resulting compounds were evaporated to powder and dried.
Synthesis of a complex compound based on Cu(II) m-hydroxybenzoate and sodium glycinate : Cu(II) An aqueous solution of benzoate (0.01 mol) was mixed with an aqueous solution of sodium glycinate (0.02 mol) in an acidic medium using a magnetic stirrer at a speed of 600 rpm at a temperature of 50 0 C for 3 hours. Received mixture filter and x left at room temperature for 15 days [12]. Product yield 82 % organization did .
[Cu(C6Ii4(OIi)COO)2* 2NH2CIi2COONa ]
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Analysis and Analysis and results. Elemental analysis and microstructure of all the synthesized compounds were determined using an Aztec Energy Advanced X-Act (Oxford) instruments brand scanning electron microscope SEM-EVO-MA 10 (Zeiss) energy dispersive X-ray spectrometer. Determination of the amount of elements in substances using a scanning electron microscope (SEM) is widely used in solving
specific scientific and technological problems due to the high information content for the analysis of materials and the reliability of the obtained research results. The amounts of carbon, oxygen and metals in the resulting complex compound were also determined by the SEM-EDA method [13].
Table 1.
The results of the elemental analysis of the synthesized initial substances and the complex compound formed
on their basis
Complex compound Cu, % C, % Na, % O, % N, %
Found Calculated Found Calculated Found Calculated Found Calculated Found Calculated
NH2CH2COONa - - 24.78 24.7 23.5 23.7 33.02 32.9 14.6 14.4
(HO-C6H4COO)2Cu 18.88 18.9 49.4 49.7 - - 28.86 28.4 - -
[Cu(CvH5O2)2 •2NaC2H4O2N] 12.76 12.8 43.51 43.2 9.13 9.2 25.92 25.6 5.44 5.6
Based on the data obtained as a result of scanning electron microscope and energy dispersion analysis, it can be concluded that the composition of the initial substances also corresponds to the theoretically calculated composition, and the coordination of metal ions with ligands leads to a change in the microstructure of ligands, in particular, many metal notes. This is confirmed by energy dispersive analysis. Thus, in the trinuclear complex compound [CuNa2Ci8Hi8O8N2] Cu (II) ions are located at the inversion center.
When analyzing the IR spectrum of the complex, changes were observed in the C=O bond of the carbonyl
group in the sodium glycinate ligand and in the NH bond in the amino group, respectively, and decreased by 16-20 cm -1 . The stretching vibrations of the CH bonds increased by 17-27 cm -1 ■ A vibration frequency in the region of 764 cm -1 , characteristic of the Na - O bond, was formed. Vibrations appeared at frequencies characteristic of the Cu-O bond at 520 cm -1 . This indicates that the carbonyl group in sodium glycinate is bonded to the oxygens and nitrogen of the amino group through a coordination bond (Figure 1).
Figure 1. IR spectrum of complex compound [Cu(C7H5O2)2*2NaC2H4O2N]
Differential scanning colorimetry is a multi-frequency analysis method with temperature modulation. As a result, the main temperature program
is modulated with wide frequencies. In terms of thermal analysis, METTLER TOLEDO's built-in DSK device measures the temperature at 800 0C. The derivatogram
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of the complex compound is presented in Figure 2, which consists of 4 curves. Analysis of the differential thermogravimetric analysis (DTGA) curve (curve 2) shows that the DTGA curve mainly consists of 1 intensive decomposition temperature range and 1
absorption range. The decomposition process occurs at a temperature of 71 -247 °C . In the second range , the substance exhibits an absorption region. This corresponds to a temperature of 280-570 ° C .
Figure 2. Derivatogram of the complex [Cu(C7H5O2)2'2NaC2H4O2N]
Analyses show that an intensive fragmentation process occurs during the first fragmentation interval. During this interval , 9.7% of the fragmentation occurs .
These derivatographic studies show that the main mass loss occurs in the range of 90-300°C, where 10.2%
Analysis of the results of the DTGA and DSC
of the main mass, i.e. 2.01 mg of mass, is lost. A detailed analysis of the differential thermogravimetric analysis curve and the DSC curve is presented in Table 2.
Table 2.
of the complex [Cu(C7H5O2^2NaC2H4O2N]
No. Temperature, o C Mass loss , % Particles of matter speed , mg/min Consumable energy quantity (^V * c/ mg )
1 50 0.425 0.124 1.40
2 100 0.685 0.365 2.00
3 200 0.925 1,784 2.14
4 300 1,035 1,257 1.78
5 400 2,285 0.214 2.02
6 500 4,569 0.874 1.45
7 600 7,815 0.411 1.59
Conclusion. [Cu(CvHsO2)2^2NaC2H4O2N] complex in the compound i Cu (II) m - hydroxobenzoate and Na glycinate each other in a ratio of 1:2 that element analysis using determined. Complex of the compound structure, in which harvest was coordination gardens IR spectroscopy method using studied. Thermal stability
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