In this paper, the results are presented by synthesizing the study of complex compounds of divalent cobalt acetate, copper and zinc with furfuryldicarbamide

Анотація наукової статті з хімічних наук, автор наукової роботи - Isakov Hayatulla


Область наук:
  • хімічні науки
  • Рік видавництва: 2018
    Журнал: Austrian Journal of Technical and Natural Sciences

    Наукова стаття на тему 'ABOUT COORDINATED COMPOUNDS OF ACETATES OF DIVALENT CO, CU AND ZN WITH FURFURYLDICARBAMIDE'

    Текст наукової роботи на тему «ABOUT COORDINATED COMPOUNDS OF ACETATES OF DIVALENT CO, CU AND ZN WITH FURFURYLDICARBAMIDE»

    ?Isakov Hayatulla,

    candidate of technical sciences, assistant professor of the Department of Chemistry, Andijan State University

    Uzbekistan, Andijan, E-mail: Ця електронна адреса захищена від спам-ботів. Вам потрібно увімкнути JavaScript, щоб побачити її.

    ABOUT COORDINATED COMPOUNDS OF ACETATES OF DIVALENT CO, CU AND ZN WITH FURFURYLDICARBAMIDE

    Abstract: In this paper, the results are presented by synthesizing the study of complex compounds of divalent cobalt acetate, copper and zinc with furfuryldicarbamide.

    Keywords: furfuryldicarbamide, metal acetates, furfural, IR spectrum, complex compounds, derivatogram, thermolysis, thermal effect.

    Numerous studies in the literature have been devoted to the synthesis and study of the properties of coordination compounds of various metal salts with carbamide and its derivatives [1; 2]. Coordination of the apical ligands is in many cases carried out through the oxygen atom of the carbonyl group. The furfuryl- dicarbamide molecule contains 7 donor atoms - three oxygen atoms and four nitrogen atoms of primary, secondary amine groups and can form complexes, with metal salts exhibiting a competitive ability for coordination of the metal with acidoligands and water molecules [3].

    Objects and methods of research

    This report describes the results of the synthesis and study of the physicochemical properties of coordination compounds of acetates of bivalent cobalt, copper and zinc with furfuryl dicarbamide (L).

    Synthesis of coordination compounds was carried out by the interaction of saturated aqueous solutions of the corresponding metal acetates and furfury ldicarbamide in a molar ratio I: I with subsequent precipitation of powder precipitates.

    Analysis of synthesized compounds on the content of metals was carried out according to [4], nitrogen by micromethod DUMA [5], carbon and hydrogen by burning in an oxygen current.

    To establish the individuality of the complexes, radiographs were taken on a DRON-2 installation with a C-antikatode [6].

    IR absorption spectra of furfuryldicarbamide and the resulting compounds in the 400-4000 cm-1 region were recorded on an IR-Fourier spectrophotometer system 2000, firm Perkin Elmer using the method of pressing samples with KBr.

    The thermal analysis was carried out on a de-rivatograph of the Paulik-Paulik-Erdei system, at a rate of 10 deg / min with a 0.1 g sample with a sensitivity of T-900, TT-100, DTA-1/10 , and DTG -1/10 galvanometers. The holder was a platinum crucible with a diameter of 7 mm without a cover. Al2O3 was used as a reference.

    Results and their discussion

    The results of the elemental analysis of complex compounds are given in (Table 1).

    Table 1.- Results of elemental analysis

    Compound M% N% C% H%

    Found Calcu. Found Calcu. Found Calcu. Found Calcu.

    1 2 3 4 5 6 7 8 9

    Furfuryldicarbamide (L) - - 28.41 28.28 42.53 42.42 5.11 5.05

    1 2 3 4 5 6 7 8 9

    Co (CH3COO) 2-L-3H2O 13.69 13.77 12.95 13.08 31.03 30.84 5.16 5.14

    Cu (CH3COO) ,. L.H2O 16.04 15.97 13.99 14.07 33.40 33.17 4.39 4.52

    Zn (CH3COO) 2-L-2H2O 15.80 15.68 13.51 13.43 31.70 31.65 4.77 4.84

    Comparison of X-ray diffraction patterns of compounds shows that they differ from those of the initial metal acetates and furfuryldicarbamide, therefore, the complexes have individual crystal structures.

    Some vibrational frequencies in the IR absorption spectra of the uncoordinated furfuryldi-carbamide molecule and its complexes with Co (II), C (II) and Zn (II) acetate are given in Table 2.

    The assignment of the absorption bands of the furfuryldicarbamide molecule was carried out according to [7-10].

    Comparison of the free molecule of furfuryldi-carbamide and its complexes with metal acetates shows, that in the transition to complexes an essential change is observed in the bands ofvalense vibrations of the ether bond -C-O-C- furan ring.

    The high-frequency shift of the valence vibration of & (-C - O - C): by 7-9 cm The sixth coordination site is filled with a water molecule-1 and the preferential valence vibration of the C = O bond by 3-4 cm-1 indicates a simultaneous participation in the coordination of the oxygen atom of the furan ring and two nitrogen atoms of substituted amine groups.

    Analysis of the values ​​of the frequency 3 (C - C) acetate group shows that in the complexes each

    group is coordinated monodentately with the participation of a ring oxygen atom in the hydrogen bond. The sixth coordination place is filled with a water molecule.

    Derivatographic data of the thermolysis of furfu-ryldicarbamide of its complexes with cobalt, copper and zinc acetates are given in (Table 3).

    The endothermic effects at 142, 220 and exothermic effects at 165, 200, 320, 490, 590, 650 ° C appear on the heating curve of the derivatogram of furfuryl dicarbamide.

    The first one corresponds to the melting of an organic ligand. The presence of subsequent thermal effects is due to the stepwise decomposition and combustion of the thermal decomposition products of substituted carbamide molecules.

    Conclusion

    The thermal behavior of coordination compounds depends on the nature of metals and is characterized by dehydration, deactivation, stepwise decomposition and burning of thermal decomposition products.

    On the basis of elemental, X-ray phase, derivatographic analysis and spectroscopic data, the following possible structure should be proposed:

    Table 2. - Some characteristic frequencies (cm-1) in IR absorption spectra of furfuryldicarbamide and its complexes with acetates of divalent cobalt, copper and zinc

    Furfuryldicarbamide - L Co (CH3COO) 2.L.3H2O Cu (CH3COO) 2LH2O Zn (CH3COO) 2L2H2O

    fre-quen-cies absorption fre-quen-cies absorption fre-quen-cies absorption fre-quen-cies absorption

    3449 ^ as (NH2) 3536, 3424 9as (OH) HA 3570 3470 9as (OH) HA 9as (NH2) 3530, 3460 9as (OH) HA 9as (NH2)

    3348 5s (NH2) 3348, 3257 9s (OH) H2O, 25 (NH2) 3424, 3335 9s (OH) H2O, 25 (NH2) 2. 3430, 3335 9s (OH) H2O, 25 (NH2), 9 (NH2)

    3140 9 (CH) f.r. 3112 9 (CH) fr. 3110 9 (CH) fr. 3111 9 (CH) fr.

    Тисяча шістсот шістьдесят шість 9 (CO), 5 (NH2) 1670 9 (CO), 5 (NH2) 1669 9 (CO), 5 (NH2) 1670 9 (CO), 5 (NH2)

    Тисяча шістсот тридцять одна 9 (CO), 5 (NH2) 1628 5 (NH2), 5 (HOH) 1627 5 (HOH), 5 (NH2) 1629 5 (HOH), 5 (NH2)

    1594 1574 5, 9 (COC) K asv 1479 9, 9 (COO) k asv 1601 9as (CO °)

    Тисячу п'ятсот тридцять шість 5 K 1603 9as (COO) 1557 9 K

    Тисяча чотиреста шістьдесят шість 9 (CN) 1441, тисяча чотиреста тридцять шість 1417 9 (CN) +9 3 (COO) тисяча чотиреста тридцять шість 1416 9 (CN) одна тисяча чотиреста п'ятьдесят шість 1417 9 (CN), 9 s (COO)

    1377 5 (CH) 1344 5 (CH) 1355 5 (CH) 1378 5 (CH)

    1310 5 (CH)

    1253 1229 9 (-C-O-C-) 1256 1236 9 (-C-O-C-) 1258 1236 9 (-C-O-C-) 1257 тисячі двісті тридцять вісім 9 (-C-C-C-)

    1149 P (NH2) тисяча сто п'ятьдесят-вісім P (nh2) 1181 P (nh2) 1180 P (nh2)

    Тисяча сімдесят сім 9 (CN) + тисячу п'ятьдесят-сім 9 (CN), 1049 9 (CN) + одна тисяча сорок сім 9 (CN) +

    1010 + 9 (-C-O-C-) 1023 9 (-C-C-C-) 1032 + 9 (-C-O-C-) 1018 + 9 (-C-C-C-)

    960 9 (CC) acet. 950 9 (CC) acet. 953 9 (CC) acet.

    884 9 k (fur.r.) 895 9 k (fur.r.) 893 9 k (fur.r.) 895 9 k (fur.r.)

    744 5 (NH2) 753 5 (NH2) 783 5 (NH2) 780 5 (NH2)

    671 617 5 (COO) 685 5 (COO) 692 5 (COO)

    559 5 (C) 527 5 (NCN) 629, 615 549 5 (NCN) 622 551 5 (NCN)

    Table 3.- Derivatographic data of thermolysis of furfuryldicarbamide and its complexes with acetates divalent cobalt, copper and zinc

    Compound Temperature effect interval, ° C Peak effect, ° C Loss of mass, Cu,% Total weight loss, Cu,% Nature effects The resulting compound

    1 2 3 4 5 6 7

    Furfuryldicarbamide (l) Removal of the hydrate molecule of water 130-143 142 0.05 0.05 endothermic furfuryldicarbamide

    143-182 165 2.27 2.32 exothermic decomposition start

    182-205 200 5.68 8.00 exothermic intensive decomposition

    205-280 220 32.95 40.95 endothermic thermolysis

    280-420 320 30.11 71.06 exothermic Thermolysis and combustion of thermolysis products

    420-542 490 21.59 92.65 exothermic decomposition

    542-595 590 6.80 99.45 exothermic decomposition

    595-770 650 0.40 99.85 exothermic Burning thermolysis products

    Co (CH3COO) 2 • L.3H2O 60-105 90 3.52 3.52 endothermic Removal of the hydrate molecule of water

    105-160 120 8.69 12.21 endothermic Removal of coordinated molecules

    160-180 175 2.72 14.93 endothermic The decomposition of the anhydrous complex began

    180-212 210 1.96 16.89 endothermic decomposition

    212-258 245 2.72 19.61 endothermic decomposition

    258-320 300 7.06 26.67 endothermic decomposition

    320-380 350 17.39 44.06 exothermic decomposition with combustion of

    Cu (CH3COO) 2 -. (L) .0,5H2O 380-510 465 22.28 66.34 exothermic decomposition with combustion of thermolysis products

    510-890 880 3.05 69.39 endothermic decomposition of cobalt carbonate

    100-130 125 2.06 2.06 endothermic dehydration

    130-155 150 2.50 4.56 endothermic dehydration complex

    155-185 170 7.60 12.21 endothermic the beginning of decomposition of anhydrous complex

    Zn (CH3COO) 2 -. (L) .2h2o 185-235 230 34.78 46.99 endothermic intensive decomposition

    235-275 278 13.04 60.03 exothermic decomposition

    275-325 290 -0.30 59.73 exothermic oxidation of thermal decomposition products

    325-380 345 -0.60 59.13 exothermic oxidation of thermolysis products

    1 2 3 4 5 6 7

    380-500 440 -0.50 58.63 exothermic oxidation of thermolysis products

    100-140 130 9.00 9.00 endothermic of education Zn (CH3COO), - L

    Zn (CH3COO) 2 -. (L) .2H2O 140-182 150 11.58 20.58 endothermic the beginning of decomposition of anhydrous complex

    182-250 210 19.28 39.85 endothermic intensive decomposition

    250-320 258 24.68 60.54 endothermic thermolysis

    320-410 380 6.02 66.56 exothermic thermolysis of a combustion product decomposed

    410-480 430 2.89 69.45 exothermic Thermolysis and formation of zinc oxide

    References:

    1. Sulaimankulov K. "Compounds of carbamide with inorganic salts" - Frunze: hahm.- 1976.- 223 p.

    2. Azizov T. A., Mahmudov Zh.U., Sharipov H. T., Beglov B. M. and others "Synthesis and study of complex compounds of divalent metal acetates with methylenedicarbamide" // Journal Inorganic chemistry -1990.- P. 35.- No. 8.- P. 2030-2033.

    3. Askarov I. R., Isaev Yu.T., Makhsumov A. G., Kirghizov Sh.M. // Organic chemistry. Uzbekistan.-Tashkent.- 2012.

    4. npum6A n. "Complexes in chemical analysis" // - Moscow .: - HA.- 1960.

    5. Klimova V. A. "Basic micromethods of analysis of organic compounds" // - Moscow .: Chemistry. -1967.- 19 p.

    6. Kovba L. M., Trunov V. N. "X-ray Phase Analysis" // - Moscow: Moscow State University - 1976-232 p.

    7. Varlomov G. D., Jalilov A. T., "Chemistry and technology of furfuramide and its derivatives" // -Uzbekistan - Tashkent.- Fan.- 1990.- P. 8-9.

    8. Spinter E. "The vibration spectra and structures of the hydrochlorides of urea, thiourea and acetamide. The basic properties of amides and thioamides" // Spectrochim. Acta.- 1959.- No. 12.- P. 95-100.

    9. Saito Y., Machida K., Uno T. "Infrared spectra of partially deyterated ureas" // Spectrochim. Acta.-1971.- V. 27 A.- P. 991-1002.

    10. Abdurakhimova N., Isakov H., Askarov IR, Usmanov S., Azizov TA // "Coordination compounds of furfuramide with acetates of bivalent cobalt, zinc and copper" // Universum: Technical science: electronic scientific journal.- Moscow. - 2017. December.- № 12 (45).


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