Yaş yöntemle üretilen fosforik asidin füzel yağlarıyla arıtılması üzerine bir çalışma
An Investigation on the purification of wet process phosphoric acid by fusel oil extraction
- Tez No: 39206
- Danışmanlar: PROF.DR. OĞUZ RECEPOĞLU
- Tez Türü: Doktora
- Konular: Kimya Mühendisliği, Chemical Engineering
- Anahtar Kelimeler: Belirtilmemiş.
- Yıl: 1993
- Dil: Türkçe
- Üniversite: İstanbul Teknik Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Belirtilmemiş.
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 82
Özet
ÖZET Bu çalışmada, fosfat kayalarının sülfürik asit ile asitlenmesi yoluyla elde edilen kirli fosforik asitin f'üzel yağı ile ekstrakte e- dilerek arıtılması ve sodyum tripolifosfat üretiminde kullanılabile cek nitelikte saf fosforik asit elde edilmesi üzerine çalışılmıştır. Bu konu üzerinde yapılan literatür araştırmasına dayanarak saf laştırma iki aşamada gerçekleşti ri İmi ştir. önce kirli fosforik asit kimyasal bir ön temizlikten geçirilerek, içerdiği %2 oranındaki SO4, BaC03 kullanılarak tümüyle uzaklaştırılmış, %0,5 oranındaki F kizel- gur yoluyla %0,02'ye, 4,85 ppm oranındaki As ise Na2S kullanılarak 1,6 ppm 'e düşürülmüştür. Çalışmanın ikinci aşamasında ise ön temizlikten geçmiş fosforik asitin f'üzel yağı ile ekstraksiyonu incelenmiştir. Bu amaçla hacim ce %80 oranında izo-amil alkol içeren rafine füzel yağı kullanılmış tır, önce kesikli solvent ekstraksiyonu yöntemi ile karıştırma hızı, karışma süresi, sıcaklık, asitteki P2O5 oranı, füzel yağındaki izo- amil alkolün oram, fosforik asitteki safsızlıklar ve fosforik asitin füzel yağına oranı gibi değişkenlerin P2O5 ekstraksiyon verimine et kisi incelenerek en yüksek P2O5 ekstraksiyon verimini sağlayan koşul lar belirlenmiş ve bu koşullar sürekli ekstraksiyon deneylerinde kul lanılmıştır. Sürekli ekstraksiyon deneyleri Fischer çok kademeli, karıştırı- cı-çöktürücülü ekstraktörde ters yönlü olarak yürütülmüş ve kademe sayısı arttırılarak safsızlıkların giderilme oranı ve P2O5 ekstrak siyon verimi belirlenmiştir. Bu deneyler sonucunda fosforik asitin füzel yağına oranı hacimce 1/4 olduğunda en yüksek P2O5 ekstraksiyon verimine ulaşılmıştır. Oç kademeli ters yönlü ekstraksiyon sonucun da elde edilen P2O5 yüklü rafine füzel yağı yine aynı ekstraktörde su ile ekstrakte edilmiş ve sodyum fosfat tuzları üretiminde kullanı lacak nitelikte teknik fosforik asit elde edilmiştir.
Özet (Çeviri)
AN INVESTIGATION ON THE PURIFICATION OF WET PROCESS PHOSPHORIC ACID BY FUSEL OIL EXTRACTION. SUMMARY An investigation on the purification of wet process phosphoric acid by fusel oil extraction. In this study, purification of wet process phosphoric acid by fusel oil extraction and obtaining technical grade phosphoric acid were investigated. Sodium t ri polyphosphate (STPP) is for example one of the main chemical phosphates imported and consumed in large amounts in Turkey (about 30,000 t/year). It is a main additive of synthetic detergents which contains normally 20-30% STPP. Detergent grade STPP should be highly pure and the mean specifications should satisfy the following values: Although this specification is satisfied by thermic phosphoric acid, attempts are also made to produce an equivalent grade phospho ric acid from wet process product. The main process of this puri fication is the solvent extraction by suitable solvents. Wet process phosphoric acid is produced by the acidulation of phosphate rocks with sulfuric acid. Therefore it contains large amount of impurities. Typical analysis of main components and impu rities of wet process phosphoric acids are given in the following table. These impurities come from the phosphate rock itself, from the reagents used for enriching the rock, from sulfuric acid used and from the reactor linings due to corrosion of material. Some of these impurities are soluble and some of them are colloidal and settle in time and cause difficulties during filtration and storage. As it is seen from the table this acid can be used in fertilizer production but it is not suitable for STPP production. Therefore viTypical compositions of wet process phosphoric acids: Weight % p?0c 27,00-30,00 Uf 1,00- 3,70 F 1,50- 2,50 CaO 0,10- 1,26 MgO 0,22- 0,33 Fe203 0,26-2,00. Aİ203 0,28- 1,60 Na20 0,06- 0,10 K20 0,02- 0,07 Si02 0,20- 0,60 they should be removed before purification. In this study, wet process phosphoric acid produced by the a- cidulation of Magdes (Israel) phosphates (which contains 15% Mazıdağı (Mardin) phosphates) in iskenderun Fertilizer Factory of Gübre Fabri kaları A.Ş. was used as a typical wet process phosphoric acid. The chemical analysis of main components and impurities of this acid is given in the following table. Weight % P2O5 30.0000 S04 2.0070 F 0.5200 Ca 0.0052 Fe 0.0064 Al 0.0054 Cr 0.0122 Ni 0.0034 Cu 0.0015 Mn 0.0007 Si 0.0149 Organic C 0.0670 As 4.85 ppm Mg 0.0184 Basing on the literature survey, wet process phosphoric acid is purified in two steps. Normally the first step is a chemical treatment which is followed by a solvent extraction. Chemical treat ment is applied to remove sulfate, fluorine and arsenic. Sulfates are generally removed as BaS04 by the addition of BaC03, fluorine is removed as H2.SİF6 (fluorosilisic acid) and SİF4 by the addition of silicious earths like diatomaceous earth or kieselguhr. Arsenic is removed as AS2S3 or AS2S5 by the addition of BaS or Na2S. Besi des these, flocculants are added to increase the settling rate and filter aids like bentonite, perlit, linters cellulose are also added for an easy and clean filtration. The organic compounds which give brown or green colours to the acid are removed through vnadsorbtion on active carbon. For this reason, in this study İskenderun wet process phospho ric acfd was first passed through a chemical treatment. Raw BaS, technical grade BaCÛ3 and: Na2S were used to remove anions like SO?", FA and heavy metal cations like As3+. Besides these chemicals, kieselguhr was added to remove fluorine. Diatomaceous earth, linters cellulose, perlit and bentonite were also investigated as filter aids. The best results were obtained when the mixture of BaC03 and Na2S together with kieselguhr was added to impure phosphoric acid at 70°C and at 250 rpm mixing rate. The precipitate formed was filtered through a precoat under 550 mm Hg. Precoat was prepared by mixing diatomaceous earth and linters cellulose. As a result of these ex periments, 2% SO4 impurity in İskenderun phosphoric acid was elimina ted completely, 0,5 %F impurity was reduced to 0,02% and 4,85 ppm As impurity was reduced to 1,6 ppm. The phosphoric acid obtained after the chemical treatment has a technical grade to be used in the production of dicalcium phosphate which can be consumed as an additive of animal fodder. In the second step of the purification, the chemically treated acid was extracted by fusel oil. There has been many studies about the purification of phosphoric acid by the extraction with aliphatic alcohols like propyl alcohol, butyl alcohol, amy! alcohol which have limited solubilities in water. In this study, fusel oil which con tains mainly iso-amyl alcohol was used as the extraction solvent. Fusel oil is a by product formed during ethyl alcohol fermen tation from molasses and obtained as a bottom product when raw alco hol is distilled. Its colour changes from yellow to brown, it is oily and has a very strong odour. Its composition and density chan ges depending on the starting raw material and it contains small a- mount of ethyl alcohol, water, 2-15 % propyl alcohol, 15-30 % iso- butyl alcohol, small amount of iso-propyl and n-butyl alcohols and 45-90 % amy! alcohols. Since the aliphatic alcohols give azeotropic mixtures, it is difficult to obtain amyl alcohols separately. In this study, fusel oil obtained as a by product in Eskişehir Alcohol Factory was used as a solvent. Gas chromatographic analysis showed that the iso-amyl alcohol content of Eskişehir fusel oil was considerably high, changing between 79 and: 85 t by volume. Since the higher alcohols, stereols and waxes wtiicfi boil above 134°C may form emulsions with acid, the raw fusel oil was first distilled and the fraction boiling below 134<>C was used as a solvent in the ex traction. vinİskenderun wet process phosphoric acid which has been chemi cally treated was first extracted by refined Eskişehir fusel oil in a batch reactor. This reactor has a hot water jacket, a helical type glass mixer and a tap at the bottom for separating the two pha ses after extraction. Tn these experiments the effect of variables such as speed of mixer, mixing time, temperature, P2O5 concentration of acid, iso-amyl alcohol content of fusel oil, impurities of the phosphoric acid and phosphoric acid/refined fusel oil ratio (by volu me) on the efficiency of P2O5 extraction were studied. The optimum values which give the highest ?2®5 extraction were then determined. Optimum extraction conditions Which has been found is as follows. An increase in iso-amyl alcohol concentration of fusel oil resulted in an elevation of P2O5 extraction efficiency. Stripping of P2O5 from fusel oil by water was also investiga ted in a batch reactor. Effect of water/P2Ü5 loaded fusel oil ratio and temperature on the efficiency of P2O5 extraction were studied. Optimum stripping conditions which has been found is a follows. Optimum stripping conditions: Water/P205 loaded fusel oil (by volume) : 1/5 Temperature : 25°C Continuous extraction experiments were performed in Fischer's multistage mixer-settler glass extractor by countercurrent flow. The effect of number of stages on P2O5 extraction and removal of impuri ties were determined. Optimum P2O5 extraction was obtained in three stages with the phosphoric acid to fusel oil ratio of 1/4. The P2O5 loaded fusel oil was also stripped in three stages with the water to fusel oil ratio of 1/5. At the end of these experiments a tech nical grade, highly purified phosphoric acid with 18% P2O5 was obta ined. The main components and impurities of the product acid are as follows. IXComposition of product acid: PZ05 Ca Mg Cr Fe Mn Cu Pb Si Al Ba 1.25 ppm
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