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DOI: http://dx.doi.org/10.20534/ESR-16-9.10-231-233
Shamsieva Makhbuba Badrievna, senior scientific employee-researcher, Tashkent institute of textile and light industry, Republic of Uzbekistan E-mail: [email protected] Kodirov Tulkin Jumaevich, technical sciences associate, professor, Tashkent institute of textile and light industry, Republic of Uzbekistan Abdurakhmonova Pokiza Elmurod kizi, student, Tashkent institute of textile and light industry, Republic of Uzbekistan
Synthesis and identification of infrared spectroscopic ester for fatliquor leather
Abstract: Ester synthesized based on oleic acid, and isoamyl alcohol. The factors are affecting the output of the ester, such as temperature, molar ratios of selected components. Spectroscopic analysis is infrared of the ester. The ester is including available raw materials, and expands the range of natural leather fattening substances.
Keywords: ester, fattening, fatliquoring, synthetic fats, fatty acids, isoamyl alcohol, IR — spectrum, the absorption band.
Fattening — is one of the main production processes that affect the quality of the finished leather. The disposition of the interaction with the skin fatliquoring agent depends on its structure, and the structure of the fatliquoring agent.
In connection with the shortage of natural fats for the production of fattening materials and an increase in production of different kinds of soft leathers emerged the need to find sources of available raw materials, design and development of methods of converting them into components of composition for half-finished leather fattening.
Underway [1] developed a new structure for the fatliquoring of leather with synthetic sulfated fat. It is determined that the best, fatliquoring and dispersing the action in regards of dermal fibers has modified synthetic oil having a degree of sulfating 30%.
The researches have shown that the half-finished leather with different composition fattening substances differ significantly in physic-mechanical properties, and in many ways change their properties under Hydrothermal and thermic influences. Fatliquoring agent containing as the cationic emulsifier is a quaternary salt of an ester of a fatty acid triethanolamine, has environmental advantage, and gives the half-finished leather good water resistance and good plasticizing effect. It can be obtained by partial etherification of triethanolamine with fatty acids in the presence of phosphoric acid,
followed by passing the air and reaction with dimethyl sulfate or ethylene oxide. According to the conducted research offered an optimal composition for fattening the following composition: 50% oxy fat, parahlor 35%, 15% of synthetic cod-liver. Samples fatliquored this composition on sensory of organoleptic and elasto-plastic figures corresponds to the best samples treated with individual components [2-7].
To select the optimum fattening acids conducted a study on the use of fattening substances of natural origin, obtained by purification of oils and fats, waste oil and fat and hydrolysis-alcohol production.
The productions of cottonseed oil fatty acids, depending on the technological scheme and the basic methods of isolating. The main products are formed a plurality of secondary food products and wastes.
Esters are having in its structure acid or unsaturated alcohol, capable of addition reactions. And also, for the research as a second agent used fusel oils derived from hydrolysis-distillery "Biokimyo" (Uzbekistan, Tashkent region, Yangiyul city). It is known that, fusel oil is a by-product of alcohol production, its average composition of 10% ethanol, 13% n — propanol, 15% of isobutanol, isoamyl alcohol 51%, 11% mixed alcohols and water. Its main component is the isoamyl alcohol, which can form the ester compound.
Figure 1. IR — absorption spectrum of oleic acid
Section 10. Technical sciences
Acid interaction was performed with the alcohol in the ratio 1: 3 with excess alcohol in the presence of a catalyst.
The resulting ester is a pasty appearance, slightly peculiar smell, dark brown color, density p= 0.878, volatile, insoluble in water liquid, but readily soluble in most organic solvents, the boiling point
T = 115 °C. The main part of these compounds is in the saturated state, 66.25% and 33.75% unsaturated state.
To identify chemicals on the spectrophotometer were removed IR — spectra. The figure shows the IR — spectra of fatty acids (Figure 1), alcohol (Figure 2.) and synthesized ester (Figure 3.):
Figure 2. IR — absorption
Spectra unscrambled using literature facts on the absorption of the characteristic frequencies of the different groups of atoms [8-9].
The researches showed that, in all the samples in the 11502940 cm-1 is observed the appearance of absorption bands belonging to the groups CH3 stretching vibration and the pendulum.
At presented IR — spectrum (Figure 2) shows a wide band of strong vibrations of the OH group near 3360 cm-1. Compare this band with an ester can be seen that the band almost disappears and leaves a very narrow peak near 3482 cm-2 and shifted to the left.
spectrum of isoamyl alcohol
Isoamyl alcohol in and around the 1710 cm-1 meets the carbon-yl C = O group and an ester it disappears (Figure 3). The absorption bands of 1465 cm-1 treated with C-C group, and 1370-1175 cm-1 to C-O group. The stretching vibrations - CH2COOR group absorbed in the band 1750 cm-1 confirms a limit aliphatic ester due to overtones and combination tones. Band at 1726 cm-1 in samples of oleic acid vanishes completely in the ester. Very strong broad band formed in 1183 cm-1 relating to HCOOR groups. The same strong broad band at 1240 cm-1 is absorbed - CH3COOR acetate groups C-O-C vibrations in oleic acid samples (Figure 1).
Figure 3. IR — spectrum absorption based In samples ofthe ester (Figure 1) ofthe absorption bands occur in the oscillation frequency of1250 cm1 inherent R -COOR groups. The ether spectrum shows a characteristic absorption band attributable to the deformation vibrations of CH located in the area of718 cm-1.
In and around the 2876 cm-1 and 2970 cm-1 appears at the ester absorption band of CH stretching vibrations substituent. The provisions of these absorption bands like the position of the methyl and methylene groups, but the rate may be considerably shifted to three methyl and methylene groups. The band is absorbed in the 1050 cm-1 refers to the average fluctuation of O-CH2 group.
There are bands absorbed with a wave number of about 1478 cm-1, due to the symmetric and ant symmetric vibrations of
on an ester of isoamyl alcohol and oleic acid
COO-. Broadening of the shift of the absorption bands in the regions 3009, 2970, 2987 and 2876 cm-1 indicates the existence of strong intermolecular hydrogen bonds.
Bands fluctuation 2935-2987, 2876 and 1478 cm-1, respectively, and should include the asymmetric, symmetric and scissor stretching vibrations of CH2 groups. As in the investigated esters are present higher aliphatic acid fragments, the fluctuation in the spectra appears in and around 718 cm-1 corresponding to the rocking vibration of several related groups -CH2-, these vibrations also applies band at 1183 cm-1 ester.
Analysis of IR — spectra of products shows, which has been a change in the position and intensity of some of the characteristic ab-
sorption bands, with the most significant in the presence of double bonds of the CHR=CHR' is characterized by the selection of appropriate bands. The strips are arranged bending vibrations tend to Trans — isomers in the 1310-1290 cm-1, cis — isomers in the 1420-1400 cm-1. The bands are of stretching vibrations settle and cis — isomers in the 3040-3010 cm-1. The presence is in spectrum of oils and esters at 1438 cm-1 and 3009 cm-1 gives an indication ofpredominantly unsaturated compounds in the cis configuration, which is characteristic of fats, oils, and esters.
To create a more efficient fattening composition in the process of leather fatliquoring of shoe upper using an ester, this provides uniform distribution of fat on the leather structure.
For the study were taken experienced and inspection lot rawhide average weighing 17-22 kg. Shoe uppers, obtained by the typical procedure proposed composition of waste on the dye bath for black.
Fattening leathers performed in suspension drums, with the temperature at 55-60 °C, fluidic coefficients 0.8. The duration is of the process for 2 hours. The flow rate was fatliquoring mixtures in composition a total amount of 7% by weight of the wringing leather based on 100% - s fat (Table 1).
Table 1. - Consumption of fattening mixtures for fatliquoring shoe uppers
Fatliquoring agents Versions of the fattening mixtures
Control Experienced
Fish oil 20 20 -
Synthetic fat 30 -
Combined oil (Touring) 50 -
Scrapings fat - 15
Technical fat - 10
Spindle oil - 15
Ester - 60
Total: 100 100
The process of fattening experienced and control versions leather held normally. All the processes before and after the fatliquoring carried out according to traditional methods. Difficulty in carrying them was not observed.
The research accorded that skin fatliquored experienced fat mixture, on organoleptic features were better control leathers quite full, soft and with a good griffin. Grades ready experienced leather was the same as the control leathers.
In order to determine the degree of influence the composition of the oiling mixture quality leather chemical analyzes was carried out and the physical and mechanical testing of the experimental and control leather. Sample preparation and testing procedures meet the requirements of existing standards.
Physical, mechanical and chemical control and experimental leather are given in Table. 2.
Table 2. - Chemical, physical and mechanical control and experimental leathers developed using etherification
Parameter Control Experienced State Standard (939-88)
Moisture,% 13,7 14,5 10-16
Ash,% 0,31 0,28 no more 0,35
Fat Content,% 7,6 8,2 7-12
Chromium oxide,% 3,9 4,1 no more 4,3
The average thickness of, mm 1,28 1,35 1,2-1,4
Tension with the appearance of the surface layer cracks 10 MPa 1,68 1,89 no less 1,3
Tensile strength, MPa, 10 MPa 2,14 2,31 no less 1,5
According to test results shown in Table 2, it is seen that the experimental and control both leather state satisfy standard requirements.
The facts in Table 2 can be seen that indicators of the surface layer strength and leather in general, and have a higher reading of the tensile strength. These facts confirm that strength is dependent not only hides the amount of injected fat, but also on the nature of the fat, its polarity, providing improvement of physic-mechanical properties of the finished leather.
Research has shown that a fatliquoring composition based on etherification suitable for fatliquoring of shoe leather chrome tanning. Depending on the required elasticity, softness, flexibility and rigidity etherification content fatliquoring mixtures and emulsions should be regulated to a certain optimum amount depending on its structure and purpose leathers. Considering the strength characteristics of various leathers etherification optimum amount in fatliquoring mixtures should not hanged and 75%, depending on the purpose of the leather.
Compared with other fatliquors material benefit received esters are extensive and rational use of secondary and by-products of local industries. In particular, the important point is the cost of production, as we believe, based on preliminary estimates, it has a cost much lower than they are now used synthetic oil and natural fats.
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