Türkiye şelit cevherlerinin oleil sarkosin, oksin ve alkil-oksin ile flotasyonu
Flotation of Turkish scheelite ores with oleoyl sarcosine as collector and oxine and alkyl-oxine as modifiers
- Tez No: 21699
- Danışmanlar: PROF. DR. OĞUZ RECEPOĞLU
- Tez Türü: Doktora
- 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: 118
Özet
ÖZET Bu çalışma çeşitli şelit cevherlerinden şelitin flotasyonla kazanılması için yapılan araştırma ve deney sonuçlarım içermektedir. Şelitin flotasyonla zenginleştirilmesi amacıyla Uludağ volfram cevheri ve Niğde silisli ve kalsitli cevherleri deneylerde kullanılmıştır. Çeşitli flotasyon parametreleri ve kollektör ve kontrol reaktifleri denenerek kalkerli ve silisli şelit cevherlerinin optimum flotas yon koşulları belirlenmiştir. Oleil sarkosin ve 8-hidroksikinolin gibi yeni reaktifler ilk kez bu çalışmada şelit flotasyonunda kullanılarak volfram spesifik bu reaktiflerin diğer tun alışılagelmiş kollektörlere göre üstünlük sağladığı saptanmıştır. Flotasyon çalışmaları iki farklı orijinli cevherin üç ayrı tenördeki numuneleri için denenmiş ve her iki cevherin değişik tenörlü numuneleri ve tüvenanları için uygun zenginleştirme koşulları çıkarılmıştır.
Özet (Çeviri)
FLOTATION OF TURKISH SCHEELITE ORES WITH OLEOYL SARCOSINE AS COLLECTOR AND OXINE AND ALKYL-QXINE AS MODIFIERS SUMMARY This study encompasses research and experimental work on the flotation of different types of Turkish scheelite ores. Siliceous and calcitic scheelite ores from Niğde region and highly magnetic scarn scheelite ore from Uludağ region were used in the experiments. Various flotation collectors and control reagents were tried in the flotation experiments as a function of a number of parameters and the optimum conditions for siliceous and calcitic ores were in dividually determined. Oleoyl sarcosine, 8-hydroxyquinoline and alkylated 8-hydroxy- quinoline were initially used in this study to separate scheelite from quartz and calcite by flotation. Better results were obtained with these reagents compared to the conventional reagents used for flotation of scheelite. It is known that the Earth Crust contains a total reserve of 2.8 million tonnes of tungsten metal in different ore deposites and distributed in 32 countries in the world. The biggest tungsten reser ves which accounts for the 55.8% of the world's total reserve are in U.S.S.R., China and North Korea. Turkey with 65 thousand tonnes of tungsten metal reserve constitutes 2.3% total reserves of the world. The most important tungsten reserve in Turkey is found in Uludağ making up 95% of the tungsten total reserves. Despite the increasing trend for use of tungsten in industrial application in recent years, the market for tungsten historically is speculative. The consumption of tungsten has been affected by the use of uranium for military purposes and the utilization of molybdenum and other heavy metals in the manifacture of high speed steels. The methods applied in the tungsten ore beneficiation depend on the structure of tungsten mineral as well as the associated mine rals. If tungsten mineral, occurs as coarse grains size, gravity met hods are best choices as applied in many plants in the world. Due to the friable character of tungsten minerals, the tungsten losses take place in the gravity concentration circuit. The direct flotati on is widely used for the beneficiation of low-grade and fine schee lite ores which present difficulties by gravity methods. Today's present technology for the flotation separation of scheelite is. based on the selective attachment of the collector to vithe calcium ions on the mineral surface. The presence of the other common calcium minerals such as calcite, apatite, fluorite and dolo mite in the ores decreases the selectivity and in turn the recovery of flotation. The objective of this study is. to develope a reagent scheme which is selective for the tungstate (W0|) ion. A selective collector or modifying agent for tungstate ion will drastically im prove the recovery and the grade of the flotation of scheelite. This main idea was employed in two different manners in the study: a) The use of the reagents which give specific chemical react ions with the tungstate part of scheelite mineral as modifying agents in addition to the common collectors. b) Developing of a new collector which can react selectively with the tungstate part of the mineral. Oleoyl sarcosine, 8-hydroxyquinoline and alkylated 8-hydroxy- quinoline were used to perform this idea. Besides the flotation ex periments, surface reactions of pure scheelite and calcite with these reagents were also studied using infrared measurements. Three different grade of siliceous scheelite ore were floated using oleoyl sarcosine as collector: Siliceous ore from Niğde region was first hand sorted into three fractions under Ultra-violet lamp according to their scheelite content as rich, medium and low grade fractions upon crushing to about 0.5 centimeter in size. These frac tions of siliceous scheelite ore samples were then ground to -210 microns and used in the flotation experiments. The grades of these rich, medium and low WOs fractions assayed 24.6%, 3.41% and 0.32%, respectively. The studies with the rich fraction of Niğde silisic ore were conducted using oleoyl sarcosine alone. A flotation scheme consisting of one rougher and two cleaning stages at pH 7.5-8, a scheelite concentrate containing 66.25% WO3 was obtained with a 83.6% recovery. An oleoyl sarcosine concentration of 400 g/t was suf ficient even to achieve this results. The flotation of medium fraction of Niğde siliceous scheelite ore (3.41% WO3) at pH 8 using 350 g/t oleoyl sarcosine as collector and 25 g/t quebracho as depressant gave a scheelite concentrate having a grade of 71.22% WO3 at 80.0% recovery. The flotation of low grade fraction (0.32% WO3) of this sili ceous Niğde ore at pH 8, using 350 g/t oleoyl sarcosine as collector, a concentrate assaying 5.82% WO3 was obtained with a 61.8% recovery. Addition of 50 g/t qdebracho as depressant into the rougher stage increased the grade to 10.17% WO3 while decreasing the recovery to as low as to 55.4%. viiAthough oleoyl sarcosine produced better results compared to the conventional fatty acid collectors in the siliceous scheelite flotation experiments * ttie selectivity of..the reagent was not adaqu- ate for the low-grade ore sample. Uludaq region run-of mine ore containing 0.41% WO3 is charac terized as higtily magnetic scam ore. Therefore, it was not possible to obtain any satisfactory result in its direct flotation with oleoyl sarcosine and other control reagents such as quebracho and phosphates. Further experiments were conducted with the table pre-concent- rate of the tungsten plant of the same Uludağ ore. The grade of the table pre-concentrate used in the experiments was 2.24% WO3. In these flotation experiments 150 g/t oleoyl sarcosine was used as collector while 100 g/t quebracho and 50 g/t hydrosol were used as depressants in one rougher and two cleaning stages. A concentrate containing 18.73% WO3 was obtained from these experiments with 53.2% flotation recovery. Magnetite removal by magnetic separation before flotation and using four stage cleaning circuits in flotation did not. increased the grade and recovery values of final flotation concentrate to a satisfying level. The researches with 8-hydroxyquinoline and alkylated 8-hydroxy- quinoline were conducted with infrared studies besides flotation ex periments. Pure scheelite and calcite minerals were used in the in-- frared studies while the rich fraction of the siliceous Niğde schee lite ore and calcitic low-grade (0.28% WO3 and 96.3% CaCC^) Niğde scheelite ore were used in the flotation experiments. Pure scheelite sample was obtained from the Uludağ tungsten plant table final-con centrate by hand sorting the scheelite particles one by one under a ultra violet (UV) lamp. Pure calcite sample, on the other hand, was obtained from the Niğde calcitic low-grade scheelite ore by hand sorting of the scheelite free calcite particles under UV lamp. Pure mineral samples were then groud to -38 microns for the infrared studies. Infrared studies with the pure scheelite and calcite ores af ter treating of the ore samples with 8-hydroxyquinoline at pH 8 and pH 3.5 showed that 8-hydroxyquinoline was adsorbed on the scheelite surface at pH 3.5. But the adsorbtion of the reagent at pH 8 was very low on the scheelite surface whereas any adsorbtion did not occur on the calcite surface. That means that 8-hydroxyquinoline is adsorbed on the scheelite surface selectively at this pH. Since calcite dissolves in water at pH 3.5, infrared study of calcite at this pH was not employed. The use of 8-hydroxyquinoline (500 g/t} in the flotation of rich fraction of the siliceous Niğde ore (24.6% MO3J besides oleoyl sarcosine and quebracho increased the grade of the rougher concent rate from 33.7% to 50.13% NO3 and the recovery from 78.5% to 95.0%. vmThe solubility of 8-hydroxyquinoline was determined ^s 3,3 10-3 M in. water. The reagent concentration of.350-400 g/t is. sufficient for an inducing effect. The main, effect of 8-hydroxyquinoTine in the scheelite flotation is that, it selectively adsorbs on the scheelite surface and consequently prevents dhe depressing effect of quebracho on scheelite. 8-hydroxyquinoline was alkylated with pentaldehide to increase its hydrophobic character with an alkylation reaction. The alkyla-. ted form of 8-hydroxyquinoline was also used for infrared studies and flotation experiments. After conditioning of pure calcite and scheelite samples with alkylated 8-hydroxyquinoline for 45 minutes at room temperature at pH 8 and pH 3.5, infrared spectra of treated samples showed that: Alkylated 8-hydroxyquinoline adsorbs on the scheelite surface at pH 8 and shows no adsorbtion at pH 3.5. On the other hand, any adsorbtion of the reagent did not occur on the calcite surface neither at pH 8 nor at pH 3.5. That also implies that, alkylated 8-hydroxy quinoline is selectively reacting onto the scheelite surface. A calcitic scheelite ore from Niğde containing 0.28% WO3 and 96.3% CaC03 was floated using Z00 g/t oleoyl sarcosine and 50 g/t quebracho. At the end of two cleaning stages a concentrate contain ing 9.33% WO3 was obtained with 57.9% recovery. The addition of 400 g/t alkylated 8-hydroxyquinoline into the rougher stage increased the grade to 31.85% WO3 at a recovery of 70.8%. After slime removing by decantation, the pulp of this low-grade calcitic scheelite ore was conditioned with alkylated 8-hydroxyquino line for 15 minutes and then with the frother addition alone, the remaining calcite slimes was removed from the system. This additional slime removing operation resulted in a better flotation medium for scheelite flotation and a scheelite concentrate containing 56% WO3 was obtained with 70% recovery. This slime removing stage with frot her after alkylated 8-hydroxyquinoline conditioning was a good process to obtaine a proper medium for the scheelite flotation. A last stage was combined to the flotation system to increase the scheelite concentrate grade: Shaking of the concentrate obtained above on a laboratory shaking table (penning). The grade of the concentrate increased to 70.0% WO3 without decreasing the recovery below 70% with this, additional table shaking step. The overall results of the present investigation can be sum marized as follows: IXOleoyl sarcosine is a selective collector for the siliceous ores containing more than 1% MO3. Pop ores with a grade about 0,3% WO3, the selectivity of the collector is not.. sufficient to obtain high grade concentrates with high recoveries, Oleoyl sarcosine performs much better than the other collectors used in flotation tests. Quebracho, pyrophosphates and hexametaphosphates used for the depression of calcite, other calcitic minerals and quartz also depressed scheelite to a large extent. For the flotation of especially low-grade siliceous and cal citic scheelite ores, 8-hydroxyquinoline and alkylated 8-hydroxy quinoline can be used as scheelite modifiers. These reagents selectively adsorb on the scheelite surface making flotation more favourable for scheelite with oleoyl sarcosine. Altough, they do not act as collectors alone, they also help to induce the efffect of sarcosine on scheelite surface by preventing the action of quebracho.
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