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Fig. 4. Electronic-microscopic image of ceramic body heat-treated at 1100 0C
Heat-treated patterns were studied by the method of electronic microscopy (Fig. 4) at the scanning electronic microscope (SEM-EDX).
The implementation of metallurgic slag of steel-making production in the composition of ceramic body contributed to the intensification of mineral
formation and obtaining of homogenous compact structure.
Based on the obtained data, ceramic floor tile was developed and its approbation was performed at the Tashkent ceramic plant. According to all indicators, received items met the specified requirements.
References:
1. Халматов М. М., Калинин В. П. Проблемы переработки техногенных отходов//Горный вестник Узбекистана, - 2003, - № 4. - С. 10-11.
2. Козубская Т. Г. Использование техногенных отходов в производстве строительных материалов // Строительные материалы. - М.: 2002, - № 2. - С. 22.
3. Залыгина О. С., Баранцева С. Е. Утилизация гальванического шлама в производстве стройматериалов //Стекло и керамика. - Москва, - 2002, № 4. - С. 3-6.
4. Патент RU 2345039. C04B 33/138. Керамическая масса для изготовления плитки для полов /Щепочкина Ю. А. Опуб. - 20.04.2014 Бюл. - № 11.
DOI: http://dx.doi.org/10.20534/AJT-16-9.10-68-71
Salimova Nigar Azizaga qizi, Azerbaijan State University of Oil and Industry, professor, faculty of "Chemical technology" E-mail: nigar_08@mail.ru Huseynova Matanet Arif qizi, Azerbaijan State University of Oil and Industry, associate professor, faculty of "Chemical technology "
Rational utilization of wastes of sulphuric acid propylene hydration
Abstract: The alkylation reaction of benzene by fraction 140-250 0C, separated from waste of production of isopropyl alcohol by sulphuric acid propylene hydration have been conducted. The waste is the cube resi-
due of the column dehydration of diisopropyl ether-being by product of isopropyl alcohol production. The results of experiments indicated possibility production of alkylbenzenes: dodecil and pentadecil-benzenes. The structure of synthesized products have been identified on base of spectral, gas chromatography analysis and results of physical-chemical investigations.
Keywords: waste, alkylation, alkylate, alkylbenzenesulphonate.
The most prevalence among the anion synthetic washing agents the alkylbenzene sulphonates of sodium RC,H SO0Na received, which with some additives are
6 4 2 '
known as sulphonol. In industry these substances received wide use that is explained by good washing properties of alkylbenzenesulphonates in composition with active additives, low cost and excellent technological qualities. These are unhygroscopic and uncaked powders that have the great significance by it is production by the method of spraing drying which is the base in production of synthetic washing agents.
One of the stage alkylbenzenesulphonates production is production of alkylbenzens by use of different alkylating agents.
In present work by purpose expansion of more available by its raw material base cost for production of al-kylsulphonates, it is offered use as alkylatng agent the waste of isopropyl alcohol production by sulphuric acid propylene hydration.
In works [1,2] the results investigations of composition of the above-mentioned waste and method of its use have been presented. The waste of isopropyl alcohol production is the cube residue of column dehydration of diisopropyl ether received as by product of isopropyl al-
cohol production by sulphuric acid propylene hydration.
There are 76-78% of propylene oligomers (three-, tetra-, penta) in cube residue of column dehydration of diisopropyl ether of the distillation of the last and return it in process, which have been determined on base spectral, gas chromatography analysis and results of physical-chemical investigations [1, 2].
In present work the research by receiving of alkylbenzenes on base of waste of isopropyl alcohol production have been introduced.
In reaction alkylation ofbenzene as an alkylating agent the fraction 140-2500C of cube residue of the column dehydration of diisopropyl ether, containing three-, tetra-and pentamers of propylene have been used. As an catalyst the catalytic complex on base of AlCl3 have been used.
Method of experiment and analysis of received products.
The necessary device and reagents: three-throat flask by volume 250sm 3 with mechanical mixer, water bath, return cooler, dropping funnel, thermometer, dry benzene chemically pure, fraction 140-2500C of cube residue of the column dehydration of diisopropyl ether (DIE) waterless, chloride aluminium, cationit CU-2, calcinated calcium chloride.
Table 1. - Conditions of experiment conducting
Have been put in reactor mol
Benzene 2.65
Fraction 140-250 0C 0.4
Chloride aluminium 0.1
Mol correlation benzene: fraction (140-250 0C) DIE 6:1
Reaction temperature, 0C 50-55
The catalytic complex — is suspension of chloride aluminium in benzene — has been loaded in reaction flask, then the rest of amount ofbenzene, necessary for reaction according to calculation and further from dropping funnel the alkylating agent a drop at a time have been added.
After addition in reaction zone the whole amount of the fraction 140-2500C, the mixture has been mixed some more 45 minutes, then the mixture has been separated in dropping funnel on two layer: upper — hydrocarbon and lower — complex. The complex may be keep under of alkylate layer in tightly closed flask and may be used in another experiments as catalyst. Received alkyl-ate have been put current through the cationit CU-2
layer, then from purified alkylate a sample has been taken for gas-chromotography, then the alkylate have been dried and have been distillated.
Benzene and part of unreacted fraction 140-250 0C have been distillated under atmospheric pressure up to 2000C temperature, then the product have been distil-lated under vacuum, by that the following fractions have been distillated: the rest amount of unreacted fraction 140-2500C; the first fraction have been distillated. By temperature 70 0C and residual pressure 1 mm mercury column, that correspond to temperature 265 0C by pressure 760mm mercury column; the second fraction have been distillated by temperature 110-120 0C and residual
pressure 1mm mercury column, that correspond to tem- Discussion of experiments results.
perature 328-355 0C by pressure 760mm mercury col- In table 2 the material balance of one of numerous
umn. The residue in flask had a more high boiling point experiments of reaction alkylation ofbenzene by fraction
and therefore haven't been distillated. 140-2500C of waste of DIE have been presented.
Table 2. - Material balance of reaction alkylation of benzene by fraction 140-2500C of waste of DIE
Have been taken Qram %, mas. Have been received Qram %, mas. yield of alkyl-benzene
Benzene 225 69.23 Benzene 207.5 63.85 -
Fraction 140-2500C of waste DIE 100 30.77 Unreacted fraction 140-2500C 53.3 16.40 -
In all 325 100.0 I fraction of alkylbenzenes 21.7 6.68 58.96
II fraction of alkylbenzenes 37.5 11.54 54.30
Residue 5.0 1.54 -
In all 325 100.0 -
Yield of alkylbenzenes fractions from theoretically possible have been calculated according to percentage content ofthree-, pentamers ofpropylene in fraction 140-2500C of waste of DIE, equal correspondingly 33.1 and 66.9% mas. [1,2]. The material balance have been calculated on base of gas chromatography analysis, carried out on chromatograph LKHM — 8 MD in following conditions: phase-polysorb, length of column 2 metre, temperature 110-1200C. The physical-chemical properties ofalkylben-zenes (I and II fractions) have been presented in table 3. Identification of alkylbenzenes (I and II fractions) have been made on base of physical-chemical properties and spectroqram, made on apparatus FT-02.
The IR — spectrum of alkylbenzenes have been presented in figure 1.
In spectroqram the following are displayed: intensive peak 1462.72 distinctive for virbartion of aromatic ring; peak 1721.24, presenting overtones and combinative tones of benzene derivatives; peak 1377.68, is related to symmetrical deformations of alkyl groups and presenting the alkyl derivatives of benzene peak 2880-2860-is methyl group, added to benzene ring.
There is peak 1160 sm-1, is related to deformative vibrations of CH in monosubstituted aromatic hydrocarbons.
Figure 1. Spectrogram of alkylbenzenes
Table 3. - Physical-chemical properties of alkylbenzenes
Name Yield on alkylate,% mas. Mol. mas. Coefficient of refraction Pensity, kq/m3 Molecular refraction MRD
I fraction Experimental Calculated
II fraction 32.4 246 1.4589 837.3 80.19 77.62
Residue 17.6 408 1.4705 857.5 93.78 89.28
50.0 >618 - - - -
Analyzing the data of table 3 and spectrogram (figure 1) it can be suppose, that in fraction I, there is dodesil-benzene and in fraction II — pentadesilbenzene. Small difference between experimental and calculated molecular refractions to all appearances is explained by indistinct rectification by distillation with dephlegmator, in result of which, in first fraction the pentadesilbenzene is taken and in second fraction dipentadesilbenzene is taken. Presence of dialkylbenzenes is confirmed by availability on spectrogram peaks 2985.16 and 2904.41.
From literary references [3] it is known, that according to consecutive mechanism proceeding of reaction al-kylation of benzene by olefins not only monoalkylben-zenes, also di- and polyalkylbenzenes are formed and olefines polymerization take place. Received highmo-lecular compound, boiling by more high temperature, have been presented in material balance as residue.
The I and II fractions of alkylbenzenes, present itself correspondingly dodesil-and pentadesilbnezenes may be recommended as alkylating agents for synthesis of alkyl-benzenesulphonates.
Residue of reaction mass, containing according to literary references (3, 4) di-, three- and more highmo-lecular polyalkylbenzenes it is not to considered as undesirable by-product.
At present time on base of high-molecular alkylben-zenes soluble in oil sulphonates and washing additions for lubricating oils are received and therefore "rear" fractions of alkylbenzenes are also valuable product.
Conclusion
Reaction alkylation of benzene by fraction 140250 0C separated from waste of isopropyl alcohol production by sulphur acid hydration of propylene have been conducted. The waste is cube residue of the column dehydration of diisopropyl ether-being by-product of isopropyl alcohol production. The results of experiments indicated the possibility synthesis of alkylbenzenes: dodesil- and pentadesilbenzenes.
The structure of synthesized products have been identified on base of spectral, gas chromatography analysis and results of physical-chemical research.
References:
1. Salimova N. A., Shakhverdiyeva F. M., Huseynova M. A. Ecologically harmless technology of sulphur acid production of isopropyl alcohol//Engineering ecology. - Moscow, - 2004, - № 5, - P. 30-36.
2. Salimova N. A., Shakhverdiyeva F. M., Huseynova M. A. Analysis of waste of sulfur acid production of isopropyl alcohol//News of higher technical institutions of Azerbaijan. - 2005, - № 1, - P. 35-37.
3. Lebedyev N. N. Chemistry and technology of base organic and oil chemical synthesis. Publishing house. Chemistry. - Moscow, - 1988, - P. 735.
4. Paushkin Y. M., Vishnyakov T. V., Belov P. S. Practical work by oil chemical synthesis. - M. Chemistry, - 1965, -P. 341.
