Kamis, 25 April 2013

Criolite



CRYOLITE
Cryolite is a double fluoride of sodium and aluminium with chemical composition Na3AlF6. Cryolite, an uncommon mineral of very limited natural distribution was only found in large quantities on west coast of Greenland. This natural deposit was exhausted in 1987. It is an importantraw material for extraction of aluminium from alumina. It has a low index of refraction close to that of water. Synthetic cryolite is used as electrolyte in the reduction of alumina to aluminium due to non-availability of natural cryolite all over the world. Composition and properties of synthetic cryolite are the same as those of natural cryolite but synthetic cryolite is often deficient in sodium fluoride. Chiolite is another sodium aluminium fluoride mineral having the chemical composition 5NaF.3AlF3. In the beginning, the only significant Cryolite mine was in Greenland where it was mined until 1987. Man-made Cryolite rapidly emerged to replace the natural mineral and now continues to meet worldwide Cryolite needs.Technically cryolite is Na3AlF6, or Sodium Aluminum Fluoride, of the Halide group.  Synthetic cryolite is produced from fluorite. Cryolite’s alumino-fluoride chemical structure loses fluoride ions in the presence of water.  All those fluoride ions running loose not only results in very effective pesticide activity, but also leaves a toxic fluoride residue in our food supply.Cryolite has several other commercial uses. For hundreds of years this mineral was used as a flux in the smelting of ores, especially aluminum.It’s also used as a pesticide applied in powder or liquid form, from ground or aerial applications, protecting crops from insects.  The most common uses of Cryolite are on California grapes, potatoes and citrus.
Lars Ohrström
Popular fiction villains often belong to sinister organisations with obscure names, and one of the more enigmatic examples is the Cryolite Corporation of Denmark, appearing in Peter Høeg's 1992 bestselling novel Miss Smilla's Feeling for Snow. However, in addition to Høeg's protagonist Smilla Jaspersen, non-fictional heroes also have connections to the very real and important chemical named cryolite, with formula Na3AlF6. For example, Vernon Jones landing his flake hit, petrol leaking, Flying Fortress on a bog in south west Sweden in 1943, and Henry Larsen, commander of the St. Roch during a voyage through the Northwest passage in 1940, the real purpose of which was not revealed until 50 years later.
Cryolite, also known as sodium hexafluoroaluminate, is a colourless compound forming cube-like crystals consisting of aluminium 3+ cations binding six fluoride F- anions, forming octahedral like AlF63-, with smaller sodium + ions to balance the charge. Perhaps you have correctly guessed that the importance of cryolite is related to aluminium, and that the World War II connection has to do with aeroplane manufacturing. But if you think that cryolite is an important source of aluminium, think again. The aluminium content of cryolite is only 13 per cent, compared to around 50 per cent in bauxite, the major source of aluminium since industrial production begun late in the 19th century. Besides the low aluminium content, cryolite is extremely rare, possibly the only mineral on Earth ever to be mined to extinction
Bauxite on the other hand is relatively common, but to lure the metal out of the mineral on an industrial scale turned out to be tricky. Three electrons need to be added to the Al3+ ions to make them neutral and metallic, and although it was recognised early on that the way to do this was to pass an electric current through a solution of the ions - what we call electrolysis - it took some 50 years of experimenting until this was achieved. The problem is that you cannot electrolyse aluminium in water, as the electrons would combine with H+ ions, producing hydrogen gas. If we circumvent the problem by melting aluminium oxide directly, the very high melting point, 2072°C, turns out to be prohibitively expensive. This is where cryolite comes in. In 1886, both Charles Hall in Ohio, US, and Paul Héroult in Normandy, France, discovered that molten cryolite, with the moderate melting temperature of only 1012°C, easily dissolves aluminium oxide.  Thus the Hall-Héroult process was born, still in use today. The name cryolite stems from the Greek words for cold, "cryo" and stone, "lithos", and this brings us to polar hero Henry Larsen's role in this story. Aluminium started to become a major material for aeroplane construction in the 1930s, and the occupation of Denmark by Germany in 1940 made the British and its allies nervous, as cryolite was found in only one place on earth - the Ivittuu mine in southern Greenland. Under the cover of a Northwest passage journey, the only Canadian government vessel able to navigate the icy Greenlandic waters, the St. Roch under command of Henry Larsen of the Royal Canadian Mounted Police, set out from Vancouver to survey the situation, as there was fear of a German invasion. With the United States entry into the war the cryolite question was resolved by Greenland temporarily becoming a US protectorate, and the production of the Ivittuu mine increased substantially. Whether there was ever a real German plan to capture the cryolite mine, as hinted to in Peter Høeg's novel, I don't know, but the only recorded Nazi attempt on Greenland was an effort to establish a weather station with a humble invasion force of 17 that was soon discovered by the Danish Hound Sledge Patrol.Instead, the Germans set up a factory for producing synthetic cryolite next to the aluminium plant in Herøya in southern Norway. This process was rather new at the time, but Nordische Aluminium never saw full-scale production as it was the target of a successful bombing mission. Not only were the factories destroyed: of the 180 B17s dispatched in the morning of the 24th of July 1943, only one was lost. However, skilful navigation and piloting of the damaged aircraft Georgia Rebel, safely landed 1st pilot Jones and his crew on neutral ground. This was the first of over 200 such US Air Force emergency landings in Sweden during world war II.
The Ivittuu mine was depleted in 1987 and today only synthetic cryolite is used in the production of aluminium. Most commonly this artificial cryolite is obtained from calcium fluoride, also known as the mineral fluorspar, sodium carbonate and aluminium hydroxide, in a multi step process. One wonders, had this mine and rare mineral not been discovered, would chemists have been clever enough to prepare it anyway and devise the Hall-Héroult process, or would there still be aluminium plates and cutlery at French state dinners, just as in the times of Napoléon III when aluminium was worth more than its weight in gold.
v  Occurrence
A late-stage mineral in some granite pegmatites; in tin-bearing alkalic granites; a vapor-phase mineral along fractures and in the groundmass of some fluorine-rich, topaz-bearing rhyolites; in pods in a carbonatite vein cutting fenitized biotite gneiss. Also as a rare authigenic component of the marlstones and shales of the Green River Formation.

v  Association
Pachnolite, thomsenolite, gearksutite, cryolithionite, weberite, jarlite, prosopite, chiolite, microcline, quartz, fluorite, siderite, topaz (Ivigtut, Greenland); sodalite, villiaumite, eudialyte, lovozerite, natrolite, chabazite, aegirine (Mont St. Hilaire, Canada).

v  Distribution
Formerly in a large deposit at Ivigtut, southwestern Greenland. In the USA, from St. Peters Dome, near Pikes Peak, El Paso Co., in the Goldie carbonatite, Fremont Co., and the Green River Formation, Colorado; in the Round Top intrusion, Sierra Blanca Peaks, Hudspeth Co., Texas; from the Zapot pegmatite, 25 km northeast of Hawthorne, Fitting district, Mineral Co., Nevada; in the Morefield pegmatite, Amelia, Amelia Co., Virginia. From the Francon quarry,
Montreal Island, Montreal, at Mont Saint-Hilaire, and from near Saint-Amable, Quebec, Canada. From Miass, Ilmen Mountains, Southern Ural Mountains, the Khibiny massif, Kola Peninsula, and elsewhere in Russia. In the Madeira and Agua Boa granites, Pitinga region, Amazonas, Brazil.Several other minor occurrences are known.





Physical Properties and Crystallography of Cryolite

Vitreous, Greasy, Pearly
Diaphaneity (Transparency):
Transparent, Translucent
Comment:
Pearly on {001}
Colour:
Colourless, white, brown, grey, black; colourless in transmitted light.
Streak:
White
Hardness (Mohs):
Tenacity:
Brittle
Cleavage:
None Observed
Parting:
On {001} and {110}, producing cuboidal forms.
Fracture:
Irregular/Uneven
Density (measured):
2.96 - 2.98 g/cm3
Density (calculated):
2.973(2) g/cm3

Crystal System:
Monoclinic
Class (H-M):
2/m – Prismatic
Cell Parameters:
a = 7.7564(3) Å, b = 5.5959(2) Å, c = 5.4024(2) Å
β = 90.18°
Ratio:
a:b:c = 1.386 : 1 : 0.965
Unit Cell Volume:
V 234.48 ų (Calculated from Unit Cell)
Morphology:
Crystals usually cuboidal with c, , or modified by r, v, k; also short prismatic [001]. {110} faces striated [111], [111], or [110]. Massive, coarsely granular.


1.      CRYOLITEHIONITE IN THE CRYOLITE DEPOSIT
In 1902 cryolithionite was found as inclusions in cryolite in the foot of the western wall of the quarry 34 .5 m below sea level . Fig . 1 shows the first sample sent from Ivigtut the 25th of October 1902 by the mine manager Mr . E . F. Edwards . He accompanied the sample with the following report (in translation) : "A block of cryolite from the NW corner of the quarry 110' below sea level, which is peculiar because,in the center of th e block occurs a cavity filled with water-clear cryolite suspended in which the common minerals galena, siderite etc. are found. The box is marked Mineral N o 1, 1902" .
This block, now in the Geological Museum of the University of Copenhagen, is mentioned by Ussing (1904) who found that the "water-clear cryolite " was indeed a new mineral . He named it cryolithionite following a proposal by the famous Danish chemist Julius Thomsen, then director of the Cryolite Company, who found that this name emphasized the resemblance to cryolite and the considerable content of Li . In his concluding remarks Ussing (1904) stressed, however, the crystallographic dissimilarities between the two minerals and emphasized analogies between garnets and the new mineral. Crystal structure determinations (Menzer 1927, 1930 and Geller 1971 ) unambiguously demonstrated the garnet structure of cryolithionite .
In the autumn of 1903 Mr . Edwards sent further samples of the new minera l reporting that it could now be found all along the SW border of the quarry " so far onl y in spots " . We have no indications that further samples were recovered from these urroundings . The existing samples show that cryolithionite appeared as rather large areas of hexagonal outline in white cryolite, up to 17 cm across, see Fig . 1 . Scattered in thi s cryolite, isolated grains of siderite and some sulphides were present in small amounts . This and the location in the quarry taken together with reports on the development of the mine in the years 1889, 1894, 1904 and 1911 indicate that cryolithionite occurred in the transition zone between the siderite-quartz-sulphide bearing cryolite (siderite - cryolite) and a body of pure, white cryolite which was being exposed in the bottom of the western part of the pit in the first years of this century, 34 m below sea level . Bøggild (1913) pointed out that cryolithionite in the intervening years had bee n
found also in black cryolite where the white crystals of the mineral stood out quite conspicuously. These samples undoubtedly came from the mining of a peculiar variety o fthe siderite-cryolite, exposed in 1889 in the bottom of the quarry, about 28 m below se alevel .
Besides the usual impurity minerals of the siderite-cryolite, cm-sized crystals o fred-brown fluorite constituted 5 to 10% of the mass . According to a map and a profil edrawing, see Fig . 2, sent from Ivigtut to the company in 1889, and some photographstaken in the period from 1890 to 1908, this peculiar variety of siderite-cryolite (in the following named BCrbF for black cryolite with red-brown fluorite) constituted an inclined,interrupted sheet through the siderite-cryolite, the only cryolite type then exposed in the quarry . The sheet was several metres thick and about 30 to 40 metre swide and long . In the western wall it was exposed about 20 m below sea level .The red-brown fluorite in the BCrbF had been observed in 1873 by Lieutenant S .Fritz (manager in Ivigtut 1866-79) in a shaft (started in 1867 from the surface) at a depth of 28 m where mining in 1889 eventually revealed its nature as an inclined sheet ; Johnstrup (1880) mentioned the occurrence of this fluorite .
Thomsen (1904) publishd a note on gases contained in some Greenlandic minerals where he, i .a ., showed th epresence of He in this fluorite . A few years later Jarl (1910) found that the fluorite was radioactive . Pauly (1960) reported a content of nearly 0 .3% Th in the red-brown fluorite . The black colour of the cryolite is attributed to the irradiation (Pauly 1962) .Cryolithionite in BCrbF constitutes a significant part of the total number of sample sof this rare mineral in the collections kept in Denmark.

2.      INDUSTRY
Synthetic cryolites are obtained by adopting several processes. The selection of the process depends upon the availability and cost of rawmaterials. The simplest and most common method of obtaining synthetic cryolite is by reacting hydrofluoric acid with soda ash and alumina hydrate. Hydrofluoric acid is produced by reacting acid grade fluorite with sulphuric acid and by-product gypsum is obtained in this process. In the secondary reaction between hydrofluoric acid and sodium chloride brine, sodium fluoride and hydrochloric acid are produced. In the primary reaction, dry aluminium hydroxide reacts with hydrofluoric acid to produce aluminium fluoride which reacts with sodium fluoride produced earlier and forms synthetic cryolite.
Besides fluorite, by-product fluorine gas emanating from plants of phosphatic fertilizer and phosphoric acid has emerged as an important alternative source for hydrofluoric acid and other fluorine chemicals including cryolite and aluminium fluoride. Rock phosphate usually contains 7-8% CaF2. In terms of fluorine, it works out to 3-4% which is liberated at the time of acidulation of rock phosphate with sulphuric acid. Fluorine combines with silica to form silicon tetrafluoride which when scrubbed with water forms fluorosilicic acid. By recycling, 18-24% fluorosilicic acid is obtained, which serves as a raw material for manufacturing various fluoro-chemicals including synthetic cryolite. From fluorosilicic acid, fluorine values are precipitated as sodium fluorosilicate by treating it with sodium salts. Sodium fluorosilicate becomes starting point for the production of synthetic cryolite. For manufacture of synthetic cryolite from sodium fluorosilicate, two routes are generally adopted in the country. They also manufacture potassium cryolite (K3AlF6) which is a foundry flux and used in welding chemicals and explosives. The total installed capacity of aluminium fluoride in organised sector was 27,000 tonnes per annum. Production of aluminium fluoride was 11,550 tonnes in 2009-10.

3.      SPECIFICATIONS
The Indian Standard Specifications of cryolite for use in aluminium industry defined vide IS - 5893 : 1989 (Second Revision; reaffirmed 2008) are as follows:
Constituents (on dry basis) Specification

1.      F                                              53% min
2.      Na                                           31 to 34%
3.      Al                                            13 to 15%
4.      SiO2 0.                                                20% max
5.      Fe2O3 0.                                 10% max
6.      CaF2 0.                                               06% max
7.      Al2O3                                                 1.00% max
8.      SO3 0.                                     50% max
9.      P2O5 0.                                               01% max
10.  Loss on Ignition (LOI)                       0.50% max
11.  NaF/AlF3(by mass)                  1.45 max

Note:    i ) LOI is to be determined at 550OC for 60 minutes.
ii) Moisture should not be more than 0.20% when determined at 110-5OC.

Cryolite obtained as a by-product during phosphate manufacture when utilised in the aluminium industry, necessary precautions are observed as even 0.01% in the electrolyte could cause 1-1.5% reduction in current efficiency in the production process of aluminium.

4.      USES AND TECHNOLOGY
The commercial application of cryolite is confined mainly to aluminium metallurgy where it is used as electrolyte in the reduction of alumina to aluminium metal by the Hall process. Alumina is a bad conductor of electricity and its melting point is 2,348 oC. It is very expensive to carry out electrolysis at this temperature. To facilitate electrolysis, alumina is dissolved in molten cryolite as it lowers the melting point. Further, addition of certain additives such as, aluminium fluoride improve the physical and electrical properties of the electrolyte besides lowering the melting point. The amount that is added is, however, limited as it also causes reduction in electrical conductivity. Addition of fluorite (CaF2) further depresses the melting point with less adverse effect on conductivity. In contrast to this advantage, too much CaF2 raises the density of the melt closer to that of liquid aluminium metal, thus inhibiting the separation of metal from electrolyte. The substituent, sodium fluoride, though known to improve the density and conductivity, also affects current efficiency. A compromise made on all these factors has led to the following general composition of bath to be in use – 80-85% cryolite, 5-7% AlF3, 5-7% CaF2, 0-7% LiF and 2-8% Al2O3. The electrolyte bath tends to deplete AlF3 content of cryolite during the process. Hence, the composition of the electrolyte has to be adjusted regularly by addition of AlF3.
In aluminium refining, high density electrolyte capable of floating aluminium is required. For this purpose, barium fluoride can also be used to raise density. Aluminium fluoride can be used to improve current efficiency of cryolite bath.
Other metallurgical uses of cryolite are in aluminizing steel, in compounding of welding rod coatings and as fluxes. In glass, cryolite functions as a powerful flux because of its excellent solvent power for oxides of silicon, aluminium & calcium and for its ability to reduce melt viscosity at lower melting temperatures. Cryolite is used as a filler for resin-bonded grinding wheels in abrasive industry to give longer life. Sodium fluoride (NaF) or fluorosilicic acid may also be used for this purpose. Cryolite is used in certain nitrocellulosebased gun propellants required in small-calibre weapons, cannons and small & large rockets.
The future of cryolite, as it may seem, is entirely dependent upon its use in the aluminium industry. It is learnt that some US firms have registered success in their research and pilot plant tests for production of aluminium directly from the mineral bauxite without the intermediate process of reduction cell. Viability of this may probably eliminate the use of cryolite in the days to come.

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