CC BY
14Toghasharov Ahat Salimovich, Ph.D.,
Senior Researcher of the laboratory "Defoliations", Institute of General and Inorganic Chemistry of the Academy of Sciences of Uzbekistan,
Askarova Mamura Kamalovna,
Ph.D.,
Senior Researcher of the laboratory "Defoliations", Institute of General and Inorganic Chemistry of the Academy of Sciences of Uzbekistan,
Tukhtaev Saidahral
,Doctor of Chemical Sciences, Professor, Academician, Head of the laboratory "Defoliations", Institute of General and Inorganic Chemistry of the Academy of Sciences of Uzbekistan,
STUDYING OF THE SOLUBILITY OF COMPONENTS IN THE SYSTEM MG(CLO3)2-CH3COOHNH2C2H4OH-H2O
Abstract: The solubility of the system Mg(ClO3)2-CH3COOHNH2C2H4OH-H2O from the temperature of complete freezing from -56.9 up to 68.4° C is studied. The polythermal diagram of solubility on which fields of crystallization of an ice are delimited, Mg(ClO3)r16H2O, Mg(ClO3)r12H2O, Mg(ClO3)r6HO, CH3COOH, CH3COOHNH2C2H4OH and new connections Mg(CH3COO)24H2O, which are identified by chemical andphys-ical and chemical methods of the analysis is constructed.
Аннотация: Изучена растворимость системы Mg(ClO3)2-CH3COOHNH2C2H4OH-H2O от температуры полного замерзания от (-56,9) до 68,4°С. Построена политермическая диаграмма растворимости, на которой разграничены поля кристаллизации льда, Mg(ClO3)216H2O, Mg(ClO3)212H2O, Mg(ClO3)?6H2O, CH3COOH, CH3COOHNH2C2H4OHи в качестве новый фазы Mg(CH3COO)r4H2O.
Keywords: solubility, system, the diagram, concentration, crystallization, temperature, chlorate of magnesium, an acetic acid, monoethanolamine, physiologically active substances
Ключевые слова: растворимость, система, диаграмма, концентрация, кристаллизация, температура, хлорат магния, уксусная кислота, моноэтаноламин, физиологически активные вещества.
For the timely harvesting of raw cotton, it is necessary the removal of cotton leaves. The big problem of cotton growing is absence complex operating domestic defoliants, which meet to all the requirements of an agriculture. The existing containing of chlorate defoliants on the basis of chlorate of magnesium does not meet contemporary requirements to defoliant. It is known, that the defoliant action of chlorate always more or lesser degree accompanied by desiccating effect. Furthermore, they do not possess a polyfunc-tional effect [1].
As psychologists approve, subsidence of leaves begins when the level of ethylene and antiauxin connected prevails over the auxin. Therefore promising is the use as defoliants compounds which accelerate the formation of ethylene and fermentative processes in the plant organism [2, 3].
It is possible to carry to such compounds monoethanolamine salts of mono-, di- and tricarboxylic acids, such as monoethanolamine acetate. For this purpose synthesis of new of complex, "soft" operating defoliants on the basis of magnesium chlorate, monoethanolamine acetate is one of the actual problems.
For the physicochemical substantiation of the process of reception an efficient defoliant on the basis of magnesium chlorate and acetic monoethanolamine,
solubility of components in system Mg(ClO3)2-CH3COOHNH2C2H4OH-H2O in a wide temperature and concentration is investigated.
Acetic monoethanolamine was synthesized on the basis of an acetic acid and monoethanolamine, taken at the molar ratio 1:1.
The solubility of components in the system CH3COOHNH2C2H4OH-H2O is studied by us in an interval of temperatures from -50.4 to 78.0°C. The polythermal diagram of solubility of this system is characterized by presence of branches of crystallization of an ice, CH3COOH and CH3COOH • NH2C2H4OH, which intersect in two double points of coexistence of two solid phases. The first double point represents joint crystallization of an ice and an acetic acid at temperature -50.4°C and concentration of 55.6% CH3COOH• NH2C2H4OH, and 44.4 % H2O. The second double point corresponds to joint crystallization of acetic monoethanolamine and an acetic acid at temperature -26.0°C and concentration of acetate monoethanolamine 78.0% and 22.0 % of water.
Mg(ClO3)2-6H2O synthesized by the method described in work [4]. The binary system chlorate of magnesium - water earlier is studied. The data re-
ceived by us will well be coordinated with the literary [5].
Polyterm of solubility of the system Mg(ClO3)2-CH3COOH NH2C2H4OH-H2O is investigated by the visually-polythermal method [6]. For identification of solid phases have been used chemical and physico-chemical methods of the analysis. At the quantitative chemical analysis of liquid and solid phases, the magnesium - determined by volumetric complexometry method [7], the chlorate ion content was found by volumetric permanganatometry method [8], the element analysis on carbon, nitrogen, hydrogen per-fonned according to the method [9]. The thermal
gMg(ClO))ilWi %
M§(C103)2-6H20
analysis study of new phases was carried out on the system derivatograph Paulik - Paulik - Erdey [10]. Radiographs of the test compounds were recorded on a diffractometer DRON 2.0 with filtered copper radiation at a voltage of U = 40 kV, I = 20 mA, the speed of movement of the counter - 2 deg/min [11].
Solubility of components in system Mg(ClO3)2-CH3COOHNH2C2H4OH-H2O is studied by means of nine internal sections. On the basis of a polyterm of solubility of binary systems and internal sections the polythermal diagram of this system from -56.9 up to 68.4°C is constructed (Fig. 1).
CHiCOOH-HHaCaHiOH
CH3COOH
Fig. 1. The diagram of solubility of the system Mg(ClO3)2-CH3COOH • NH2C2H4OH-H2O
vra -2SU0 go к
CHJCOOH-NHÏCJH^OH, Wt%
On the polythermal diagram of solubility fields of crystallization of an ice, Mg(QO3)2^6H2O, Mg(QO3^ 12H2O, Mg(ClO3)2-6H2O, CH3COOH, CH3COOH-NH2C2H4OH and as new phase Mg(CH3COO)2 • 4H2O are determined. The specified
fields converge in three triple but alternative points of system. Double and triple points of the system Mg(ClO3)2-CH3COOHNH2C2H4OH-H2O are resulted in the table 1.
Table 1.
Double and triple points of the system Mg(ClO3)2-CH3COOHNH2C2H4OH-H2O
Composition of a liquid phase, % tcr, °C Solid phase
Mg(ClO3)2 CHsCOOH-NH2C2H4OH H2O
36,9 0 63,1 -52,0 Ice +Mg(ClOs)216H2O
31,8 9,2 59,0 -53,0 Same
25,6 22,5 51,9 -54,4 -//-
23,6 30,4 46 -54,8 Ice +Mg(ClO3)2- 16H2O+Mg(CHsCOO)2-4H2O
13,0 46,4 40,6 -56,0 Ice +Mg(CHsCOO)2-4H2O
12,4 54,8 32,8 -56,2 Same
12,2 57,2 30,6 -56,9 Ice +CH3COOH+Mg(CHsCOO)2-4H2O
10,6 57,0 32,4 -55,7 Ice +CH3COOH
8,4 56,6 35,0 -53,8 Same
3,8 56,0 40,2 -51,8 -//-
0 55,6 44,4 -50,4
12,6 65,7 21,7 12,8 CHsCOOH+MgCCHsCOOb • 4H2O
12,8 67,8 19,4 16,4 Same
13,0 69,6 17,4 19,0 -//-
13,8 74,4 11,8 23,4
14,0 76,0 10,0 25,2 -//-
11,8 79,6 8,6 28,8 C H3COOH+CH3COOHNH2C2H4OH
11,0 79,4 9,6 26,8 Same
8,2 79,2 12,6 20,2 -//-
8,0 79,0 13,0 18,0
4,2 78,6 17,2 -16,0
3,6 78,4 18,0 -22,0
0 78 22 -26,0 -//-
28,6 27,8 43,6 -19,4 Mg(ClO3)2-16H2O+Mg(CH3COO)2-4H2O
32,8 25,8 41,4 8,2 Same
36,4 24,8 39,8 24,4 Mg(ClO3)2- 16H2O+Mg(ClO3)2- I2H2O+ Mg(CH3COO)2-4H2O
37,4 24,6 38,0 26,4 Mg(ClO3)2-12H2O+Mg(CH3COO)2-4H2O
41,4 24,2 34,4 54,8 Same
41,6 24,0 34,4 55,6 -//-
44,2 24,0 31,8 68,4 -//-
36,0 22,8 41,2 20,8 Mg(ClO3)2- 16H2O+Mg(ClO3)2- I2H2O
35,6 20,4 44,0 19,2 Same
35,2 16,0 48,8 2,0 -//-
36,0 9,8 54,2 -13,2
36,6 7,4 56,0 -16,0
37,8 5,4 67,6 -19,4
42,0 0 58,0 -21,7 -//-
43,6 20,2 36,2 50,2 Mg(ClO3^ 12H2O+Mg(ClO3)2 6H2O
42,8 18,4 38,8 45,8 Same
41,8 16,6 41,6 36,8 -//-
40,2 12,6 47,2 17,0
40,3 10,0 49,7 8,6
41,0 6,0 53,0 0,8
44,6 1,0 54,4 -6,2
45,2 0 54,8 -7,5
From the diagram of solubility it is visible, that in the investigated concentration and temperature limits in the system compound of the composition Mg (CH3COO) 24H20 which is allocated in a crystal kind and is identified chemical and physicochemical methods of the analysis.
The chemical analysis of the solid phases separated from the crystallization regions of the assumed compound Mg(CH3COO)2'4H2O gave the following results:
Found, wt %: C, 22.2; H, 6.45; MgO, 18.74. For Mg(CH3COO)2-4H2O, clcd, wt %: C, 22.39; H, 6.53; MgO, 18.81. The X_ray powder diffraction analysis showed that the synthesized compound of the composition Mg(CH3COO)2-4H2O are characterized by it own values of the interplanar spacings, which confirms their individuality (Fig. 2).
Fig. 2. X_ray diffraction patterns of the compound Mg(CH3COO)2-4H2O.
The thermal analysis of the firm phase allocated from prospective area of crystallisation of connection Mg(CH3COO)2 • 4H2O has shown that on a curve of heating in the range of temperatures 20-900 °C a
number endothermic events is observed at 92, 150, 347, 401 °C and two exothermic events at 476 and 738 °C (Fig. 3).
Fig. 3. The derivatogram of the compound Mg(CH3COO)2-4H2O.
Fusion of the given connection begins with 80 °C and to it there corresponds effect at 92°C. Thus alongside with fusion there is a partial removal of water. Loss of weight makes IT = 1.98%. Following endothermic effects at 150 °C corresponds to the further removal crystallization water, loss of weight makes Tr = 28.4 %. Endothermic effect at 347 °C there corresponds to removal of the remained water and decomposition Mg(CH3COO)2 • 4H2O thus loss of weight
makes 35.78 %. Effects at 401, 476 and 738 °C corresponds to the further decomposition of connection and products of its disintegration. The general loss in weight at 900 °C 82.0 %.
Thus, the obtained data on the solubility of components in the studied system Mg(ClO3)2-CH3COOHNH2C2H4OH-H2O are by a scientific basis for reception a liquid defoliant on the basis of chlorate of magnesium and acetic monoethanolamine.
References
1. Umarov A.A., Kutyanin L.I. New defoliants: search, properties, application. M.: Chemistry. 2000. - 87 pp. (in Russian).
2. Saidov M.T. Application of ethanolamines in agriculture // Uzbek Chemical Journal. 1983. -№ 1. - pp 58 - 64. (in Russian).
3. Narhodzhaev A. Kh., Adilova M.Sh., Isakova D. Tukhtaev S. Scientific bases of synthesis of growth factors of plants from transient waste of primary processing a cotton - a raw // Materials of the International scientific-practical conference on the theme: "Scientific and practical bases of improvement of soil fertility. " - Tashkent, 2007. Part I. - P. 353-355. (in Russian).
4. Martynov J.M., Matveev M.A., Yakimenko L.M, Furman A.A. The technology of production and application of magnesium chlorate defoliants // Chemical Industry. 1958. №7. - P. 420-423. (in Russian).
5. Toghasharov A.S., Tukhtaev S. Study of the solubility of the system Mg(ClO3)2-2NH2C2H40H-H3C6H507-H20 // Journal of Inorganic Chemistry. 2013. vol. 5(58). - P. 658-662. (in Russian).
6. Trunin A.S. Petrova D.G. The visually-polythermal method. - Kuibyshev: Kuibyshev Polytechnic Institute. 1977. 94 pp. Dep. VINITI. №584-78. (in Russian).
7. Schwarzenbach G., Flaschka G. Complexometric titration. - M.: Chemistry, 1970. - 360 pp. (in Russian).
8. Tsh. 88.16-34-2010. Liquid magnesium chlorate defoliant. Technical conditions. - T.: Publishing house of standards, 2010. - 5 pp. (in Russian).
9. Klimova V.A. The main micromethods of analysis of organic compounds. - M.: Chemistry, 1975. - 224 pp. (in Russian).
10. Practical Guide to thermography / Berg L.G., Brumistrova N.P., Ozerova M.I., Purinos G.G. - Kazan: Publishing House of the University of Kazan, 1976. - 222 pp. (in Russian).
11. Kovba L.M., Trunov V.K. X-ray analysis. - M.: - Publishing House of the Moscow State University, 1969. - 160 pp. (in Russian).
Shukurov Zhamshid Sultonovich,
candidate of technical science Askarova Mamura Kamilovna,
candidate of chemical science, Tuxtaev Saiydiaxral,
doctor of chemical science, academician, Institute of General and Inorganic Chemistry of the Academy of Sciences of Uzbekistan
Шукуров Жамшид Султонович,
кандидат технических наук Аскарова Маъмура Камиловна,
кандидат химических наук, Тухтаев Сайдиахрт,
доктор химических наук, академик, Институт общей и неорганической химии АН Республики Узбекистан,
STUDY OF SOLUBILITY OF COMPONENTS IN THE SYSTEM [98,0 % NACLO3 • CO(NH2)2 + 2,0% H3PO4- CO(NH2)2] -NH2C2H4OH - H2O ИЗУЧЕНИЕ РАСТВОРИМОСТИ КОМПОНЕНТОВ В СИСТЕМЕ [98,0 % NACLO3 • CO(NH2)2 + 2,0% H3PO4- CO(NH2)2] -NH2C2H4OH - H2O
Abstract: The solubility of the components in the system [98,0 % NaClO3 • CO(NH2)2 + 2,0% H3PO4 • CO(NH2)2] -NH2C2H4OH - H2O visually - polythermal by a wide temperature range. In the phase diagram delimited field of crystallization: ice, urea, sodium monokarbamidohlorata, double, single and anhydrous mo-noethanolamine. In the studied system, there is no formation of new chemical compounds on the basis of the initial components. The system refers to a simple evtonic type.
Keywords: chart solubility polyterm system, monokarbamidohlorata sodium, urea phosphate, monoethano-lamine.
Аннотация: Изучена растворимость компонентов в системе [98,0 % NaClO3 • CO(NH2)2 + 2,0% H3PO4• CO(NH2)2] -NH2C2H4OH - H2O визуально - политермическим методом в широком интервале температур. На фазовой диаграмме разграничены поля кристаллизации: льда, карбамида, монокарба-мидохлората натрия, двух- и одноводного моноэтаноламина. В исследованной системе не происходит
