Fusel yağının Na2SO4 kullanılarak suyunun azaltılması
Removal of water from fusel oil by using Anhydre Na2SO4
- Tez No: 39370
- Danışmanlar: DOÇ.DR. DURSUN ALİ ŞAŞMAZ
- Tez Türü: Yüksek Lisans
- Konular: Kimya Mühendisliği, Chemical Engineering
- Anahtar Kelimeler: Belirtilmemiş.
- Yıl: 1992
- Dil: Türkçe
- Üniversite: İstanbul Teknik Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Belirtilmemiş.
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 114
Özet
ÖZET Sunulan çalışmada amaç, melas orijinli fusel yağının suyunun Na 2 SO 4 kullanılarak giderilmesi şartlarını incelemektir. Bu amaçla, Eskişehir alkol fabrikasından temin edilen fusel yağı, susuz Na2S04 İle, değişik sürelerde, kuvvetli bir şekilde karıştırıldı. Sonra bu karışım vakum altında süsülerek, bünyesine su almış Na2S04 partikülleri ile suyu azaltılmış fusel yağı birbirin den ayrıldı (şekil 4-1). Daha sonra, bu elde edilen fusel yağı, basit distilasyon işlemine tabi tutularak, belirli hacimlerde fraksiyonlarına ayrıldı. 82*0-132*0 sıcaklık aralığında alınan bu fraksiyonların her birinin su, etil alkol, normal propil alkol, iso butil alkol ve izoamil alkol içerikleri, gaz kromatografisi yöntemi ile belirlendi. Yapılan 25 tane denemenin ayrıntılı değerleri tablo 4-2 'de verilmiştir. Tablo 4-4 "de ise, deneysel delerlerden yararlanılarak hesaplanan, başlangıç ve son su miktarları ile su çekmede kullanılan fusel yağı içindeki NasS04 ağırlıkları görülmektedir. Bu değerlere göre 900 cm3 fusel yağı içinde bulunan 93.2 gr su, 125 gr Na2S04 ile 2 saatlik bir kuvvetli karıştırma sonunda 57.9 gr değerine düşürülmüş, yani fusel yağı içindeki suyun; 93.2-57.9 -% 38 93.2 miktarı giderilmiştir. Su miktarının, daha fasla HasSCM kullanılarak ve karıştırma süresi artırılarak daha asa indirilmesi, uygun görülmemektedir. Çünkü hem NasS04 in tuttuğu fusel yağı miktarının artmasıyle hammadde kaybedilmekte, hemde karışımın süzülerek katı ve sıvı fazların ayrılması güçleşmektedir. Fusel yağından suyun alınması içindeki alkollerin daha düşük sıcaklıklarda distillenmesini sağlamakta, bunun yanında alkol miktarlarında bahse değer bir değişime sebep olmamaktadır. VI
Özet (Çeviri)
SUMMARY Removal Of Water From Fusel Oil By using Anhydre Na2S04 I nt roduc t ion The aim of this work is decreasing water content or dehydrating of fusel oil which is the residue of alcohol plant. Fusel oil used in the experiment is taken from Eskişehir alcohol plant, which is located on middle Anatolia in Turkey. Properties Of Fusel Oil Fusel oil is volatile, poisonous with disagree able odour, oily mixture and consisting of largely amyl alcohols. Ieo amyl alcohol is main constituent. Ethyl, propyl and iso butyl alcohols as well as other alcohols have been separated. The only natural re sources of C3/C5 alcohols is fusel oil. However, it is possible to produce these alcohols with synthesis. Fusel oil which is obtained as a by product in the alcoholic fermentation of molasses in Eskişehir is a clear liquid and has a light brown color. It has the density of 0.845 gr/cm3 and %19.74 water content by weight. Pure alcohol fraction of fusel oil consis ts of amyl (%76), iso butyl (%5), propyl (%3) alcohols water and other minor components (%16). Usage Of Fusel Oil ±n Industrie Manufacturing of chemicals (amyl ether, amyl ace tate, pure amyl alcohols nitrous ether varius esters). Preparation, identification and prufication of alkoloids in analytical chemistry, manufactures of ex plosives as a gelatinising agent, solvent of fats and oils artificial fruits groups, solvents of resins and waxes, and in parfumery Industrie. VIIBrief Dieeription Of Gas Chromatography Gas chromatography is a process in. which the com- ponents of a mixture are separated fro» one another by volatilising the sample into a carrier gas stream which is passing through a bed of packing consisting of a 20 to 200 mesh solid support. Different components which are present in the sample, pass through the bed of packing at different rates and so appear one aftei* the other at the eff luent end, where there are detected, determine and measured by thermal conductivity changes, density dif ferences, oi* various types of ionization detectors. Experimental Study Experiments for fusel oil, has been ( fig 1 and table 1 ). decreasing of carried out in water fro» crude the following way 900 c»j3 of crude fusel oil, which has the density of 0.846 g/em3 and %19,74 by weight water content, has been added m g anhydre KasS04 and Mixed strictly, with a certain period. Mixing time for different experi ments are chosen 0.5, 1 and solid liquid mixture is left ly is filtered in vacuum. 2 hours. After that, the for decantation and final / itov Pcw#r Rtdut for I BrSHer m m J cm hitel ml « re H ae I- eu.a a. m.1 =. -a *~i «-.4 CO cm i~. t-- *~l cm o -a o.-i cm ?»-.I era cm |-“J CO r-j ca CO o o Cr- CI-. CO cm o.-I ca ca cm ca cm r-i to to rmrfmwttnittt, ittrfwwtaww rennti'öKivıt to.J3 l»-J !!«*? I >u >lj tjul Hl'illlHim iiiJUMIIiiUji. m Cİ Cİ' ?J3 ca.J3 CM CO CM O CO »a -a IXafter filtration, Mı gr of solid phase and V cm^ dehydrated fusel oil ax~e obtained. Solid pahse which is a mixture of NaaSCU, water and a little part of crude fusel oil, is wasted. 500 cms of fusel oil, in which watei”content is reduced, is put into a distil lation flask and separate into fractions. This simple distillation, starts 74“C and continuous to 132”C Quant itave analysis of withdrawal 1 fractions has been made by gas chromatography. Conditions Of Gas Chromatographic Determination Device and dedector type : Hawlett Facfcard-5890, TCD Injection temperature : 180 °C Initial Oven temperature : 185 °C (waits 4 min) Oven temperature increasing rate : 10°C/min Final Oven temperature : 205 °C Column characteristics : Chr-omosorb 101, 80-100 mesh, 3 mm ID * 2 m length Carrier Gas and its Flow rate : Hydrogen, 20 ml/min. Quantity of Sample : 0.3 nl. A typical chromatogram is show in figure 2. JİY^1 jP^AJ rs; r #R8 Frak 1 Frak 2 Frak 3 Frak 4 Frak 5 Figure 2. Choromatogram Obtained From Fractions Of Experiment 20 (D 20) The results of chromatographic analyses are shown in table 2. XTable 2 Boiling Point Range, Voluae, Hithdra*mll Tite and ZH Cosposition of Fractions (Only for Exp. 21 and Exp. 22. Others are in the Turkish Text) Retention time of various alcohols, which are constituent of fraction, are shown in below. XIYield Of Dehydration Operation Yield of dehydration operation has been defined as the quantity of i~erooved water (g) from ca-ude fusel oil divide by amount of anhydride N&2SQ4 (g); Removed Water (g) Yield- Used Anhydrite N&2S04 (g) Yields of each experiment, which from above definition, is shown in the Table 1. Yield curves has been drawn lues, taken mixing time as parameters, are shown in figure 3. is calculated last column of from these va- These curves Results and Discussions 1- It is possible to remove a certain quantity of wa ter from crude fusel oil. For this dehydration opera tion one hour stirring and use 0.15 g of anhydride NasS04 per em3 of crude fusel oil as a dehydration a- gent is sufficient. 2- By working with these conditions, water content of crude fusel oil can be reduced to %9 from %20, based on weight composition. 3- It is not necessary to decrease much lower the wa ter content with using much more NasS04. Because, in creasing of NasS04 increases the holding of fusel oil in the solid phase. Thus, much more raw material has been wasted. At the same time, filtration operation can be made with an increasing diffuculty. 4- Dehydration of crude fusel oil causes to boiling point decrease. Therefore distillation of dehydrated fusel oil is performed in lower temperature, providing some amount heat or en&rgy saving (Figure 3). 5- It is not seen a remarkable difference from point of amount of alcohols between dehydrated and crude fu sel oils. XII140 130 120 ou 110 a 100 E.1> 90 80 70 50 100 150 200 250 300 350 400 Distilat Velum» feci Figure 3. Comparison Of Simple Distilation Curve Of Crude Fusel Oil To That Of Dehydrated Fusel Oil XIII
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