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Manufacture of Aluminium Fluoride of High Density and Anhydrous Hydrofluoric Acid from Fluosilicic Acid

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Manufacture of Aluminium Fluoride of High Density and Anhydrous Hydrofluoric Acid from Fluosilicic Acid Available online at www.sciencedirect.com Procedia Engineering 46 ( 2012 ) 255 – 265 1st International Symposium on Innovation and Technology in the Phosphate Industry [SYMPHOS 2011] Manufacture of Aluminium Fluoride of High Density and Anhydrous Hydrofluoric Acid from Fluosilicic Acid Alain Drevetona,* AD Process Strategies Sarl, Rue Chaponnière 9, CH-1201 Geneva, Switzerland Abstract New process technologies are disclosed to manufacture aluminium fluoride of high density and anhydrous hydrofluoric acid starting from fluosilicic acid as raw material which is obtained during acidulation of phosphate rock in the manufacture of phosphatic fertilizers. An overview of the relevant process technologies used commercially to consume this fluosilicic acid is provided in this paper. The new process technologies which shall be implemented to satisfy market demand in fluorochemicals (production of aluminium fluoride of high density from fluosilicic acid and production of anhydrous hydrofluoric acid from fluosilicic acid) and overcome some technical issues as well are described. © 2012 TheThe Authors.Authors. Published Published by by Elsevier Elsevier Ltd. Ltd. Selection Selection and/or and/or peer-review peer-review under under responsibility responsibility of the of theSelection Scientifi and c /or peer-reviewCommittee ofunder SYMPHOS responsibility 2011 of the scientific committee of SYMPHOS 2011. Keywords: aluminium fluoride, hydrofluoric acid, fluorine technology, fluosilicic acid, fluorochemical, silicon tetrafluoride, sodium silicofluoride, suplphate of potassium, sodium sulphate Nomenclature AHF Anhydrous hydrofluoric acid ATH Alumina trihydrate, aluminium hydroxide DCP Dicalcium phosphate FSA Fluosilicic acid, fluorsilicic acid FSA1G FSA-based technology of the first generation FSA2G FSA-based technology of the second generation FSA3G FSA-based technology of the third generation HBD High bulk density, HD-AlF3 HFC Hydrofluorocarbon KSF Potassium silicofluoride, Potassium fluosilicate LBD Low bulk density, LD-AlF3 MGSF Magnesium silicofluoride, Magnesium fluosilicate MOP Muriate of Potassium, KCl PA Phosphric acid PR Phosphate rock, Rock SA Sulphuric acid SAC Sulphuric acid concentration * Corresponding author. Tel.:+00 41 22 548 1249; fax:+00 41 22 545 7512. E-mail address: [email protected] 1877-7058 © 2012 The Authors. Published by Elsevier Ltd. Selection and/or peer-review under responsibility of the Scientifi c Committee of SYMPHOS 2011 doi: 10.1016/j.proeng.2012.09.471 256 Alain Dreveton / Procedia Engineering 46 ( 2012 ) 255 – 265 SSA Sodium sulphate anhydrous SSF Sodium silicofluoride, Sodium fluosilicate SOP Sulphate of Potassium STF Silicon tetrafluoride Symbols MMT Million metric tons 1. Fluorine raw material resources Fluorochemicals are essentially produced from raw material fluorspar (Acid Grade Fluorspar: CaF2 > 97%). A small amount only (about 5%) is produced from phosphate rock, an alternative raw material containing fluorine for production of: • Fluosilicic acid • Fluosilicates • Cryolite • Aluminium fluoride • Silicon tetrafluoride 1.1. Uses of Fluosilicic acid Fluosilicic acid is used as water fluoridation agent of drinking water to prevent tooth decay in US, Canada, South Africa and Australia mainly. The US production of fluosilicic acid in 2010 estimated and reported by USGS (Miller, 2010) is 68’000 tons (FSA as 100% H2SiF6) mostly used for water fluoridation and manufacture of silicon tetrafluoride (STF = SiF4) up to 20’000 tons being a raw material for polysilicon produced by MEMC, an intermediate to high purity silicon for solar and chips applications. In this process, MEMC claimed that the capital cost of this process is reduced by 50 % compared to classical Siemens process and electric consumption for purification reduced by 20 folds. Other uses of FSA are in the tanning of animal skins, in ceramic and glass etching, in technical paints, in oil well acidizing, preservative of wood, hardening of masonry, remover of mould, remover of rust and stain in textiles, cleaning and sterilizing agent in industry, and in electro-refining of lead, etc. Very minor quantities of FSA are produced also from fluorspar processing. Table 1: Uses of fluosilicic acid FLUOROCHEMICAL YEARLY CAPACITY COUNTRY COMPANY PRODUCT (TON) US 4 Companies (Plants) Reporting FSA << 68’000 US PCS Phosphate Co. STF < 28’000 EU (BE) Prayon SSF/PSF 18’000 / 3’000 EU (HU) Bige Holdings Cryolite << EU (PL) TARNOBRZEG Ltd. Cryolite << EU (SE) Alufluor LD-AlF3 23’000 CN Several Producers LD-AlF3 Small CN Wengfu AHF 20’000 IN Alufluoride LD-AlF3 5’000 IN Hindalco LD-AlF3 3’000 SSF/PSF/MGSF CN Several Plants -- /NH4F CN Yunnan Three Circles Chemical Industry Co. SSF/PSF -- JO JPMC LD-AlF3 20’000 ID PT Petrokimia Gresik LD-AlF3 12’000 RU Phosagro /Ammophos LD-AlF3 / SSF 23’000 BY JSC Gomel Chem. Plant Cryolite / LD-AlF3 5’000/5’000 LT Eurochem / Lifosa LD-AlF3 17’000 Alain Dreveton / Procedia Engineering 46 ( 2012 ) 255 – 265 257 Aluminium fluoride is still the major product out of FSA with a production < 100’000 tons / annum against about 800’000 tons / annum mainly produced from fluorspar reported by (Reynolds, 2010) . See Table 2 below. Table 2: World and China aluminium fluoride (AlF3) production and consumption per year (x 1’000 tons) STF could grow significantly as its added value is higher than manufacturing AlF3 / AHF making projects even more attractive. Already five projects have been implemented in Asia (approx. 70’000 tons / annum STF) using the fluorspar process although it makes more sense to start from FSA. Presently there is a supply shortage of FSA for water fluoridation in US and Canada and prices of FSA have risen significantly. 1.2. Fluorspar resources China is dominating largely the fluorspar industry (59% of world fluorspar production) (Will, 2010)) and China is starting to face sourcing problems at present. China has changed its policy with tighter rules. Consequently fluorspar prices are rising. Europe has included fluorspar in a list of 14 minerals classified as “critical”. A raw material is labelled “critical” when the risks for supply shortage and their impacts on the economy are higher compared with most of the other raw materials a) (b) Fig. 1 : World production of fluorspar (a) 5.1 million tons (Will, 2010) and (b) 5.4 million tons (Miller, 2010). Reserves of fluorspar are reserves that are economical to extract and recover according to USGS (Miller, 2010) are also reported. According to (ResearchInChina, 2010), the fluorspar reserves in China (2009) reached 21 million tons, providing 9.3% of the world’s total, ranking at the third position, while the fluorite output recorded three million tons in the same year, contributing 58.8% to the world’s total, topping the global list. According to statistics of year 2009, the ratio of fluorite 258 Alain Dreveton / Procedia Engineering 46 ( 2012 ) 255 – 265 reserves to output in China was not more than seven, indicating that the fluorite resource in China is likely to run out within seven years provided that the recoverable reserves of fluorite will fail to increase. China is deficient in fluorite resource and demand is growing for fluorite year after year at significant pace. In 2009, the apparent consumption of fluorite in China reached 2.8 million tons, up 8.2% from a year earlier; and the figure in H1 2010 hit 1.93 million metric tons (MMT). Concerning the consumption of fluorite, China ranks first around the globe, but lags far behind the developed countries in term of downstream consumption. A case to this is fluorine chemical industry, the demand of fluorite is 30% less in China than opposed to nearly 60% in developed countries. Fig. 2 : Map of fluorspar reserves in China (HeQing, 2005, p. 5) (a) (b) Fig. 3: World HF production capacity is about 2 million tons in 2009 (a) and Fluorine Industry Segments: fluorocarbon production is the largest HF segment followed by aluminium fluoride production (Will, 2010) As long as fluorspar was cheap, there was no need for an alternative source of fluorine like FSA. Presently the price of fluorspar is about USD 350.-/ton FOB compared to FSA 100% that can be produced very cheaply, by operating a single absorber. The theoretical price of FSA would be USD 600.-/ton if fluorine F contained in FSA is assumed at the same value of F contained in fluorspar. At this price, it makes any business for fluorine attractive and it is adding appreciable value to the phosphate business. Especially for aluminium fluoride that is a bulk chemical, easily transportable requiring large Alain Dreveton / Procedia Engineering 46 ( 2012 ) 255 – 265 259 amounts and competitive sources of fluorine. At the time of writing this paper, some Acid Grade Fluorspar from China reached USD 500.-/ton back to pre-recession highs. • phosphate rock resources The world population is expected to reach 9 billion of inhabitants in 50 years and productions / capacities are forecasted to increase by more than 50% maybe 70%. In the near future, fluosilicic acid uses will probably increase bearing in mind that environmental regulations are more stringent, technical hurdles for the technology are now resolved, technical expertise is available, communication between the industrial sectors concerned is improving constantly. The phosphate rock reserves are assumed to be sufficient for more than a century; other base reserves less attractive will be considered at the end of the century only. (See below Fig. 4 Hubbert peak for phosphorus) Table 3: Phosphate rock production and reserves according to USGS (Jasinski, 2011) According to International Fertilizer Association (IFA, 2009), the world production of phosphate rock in 2009 was 162 million tons phosphate rock (49.7 million tons as P2O5) and the world production of phosphoric acid was 33.6 million tons expressed as P2O5 (48.6 million tons expressed as H3PO4) Assuming that phosphate rock contains 2 to 5% fluorine (average approx. 3% F) an amount of 4.8 million tons of fluorine is available which is about twice the amount of F present in fluorspar. (Fluorspars are up to 48% F).
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