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Mineral Acids Course : ACCE-2221 2nd Year : Even Semester Group-A : Chapter-1 7 December 2015 Course Outline 1. Sources of sulphur 2. Mining of sulphur- Sicilian and Frasch processes 3. Manufacture of sulphuric acid- chamber and contact process 4. Oleum and uses 5. Production of hydrochloric acid and nitric acid- Properties & uses 7 December 2015 Mineral Acid A Mineral Acid is an acid derived from one or more inorganic compounds. One part of these acid comes from inorganic minerals, that is why these acids are known as mineral acid. Some mineral acids are- • HCl • HNO3 • H2SO4 • H3PO4 • H3BO3 • HClO4 • H4TiO4 7 December 2015 Sources of Sulfur • Volcanic deposits in Sicily (Italy) • Iron pyrite • Ammonium sulfate • Calcium sulfate • Fossil fuel • Zinc blend • Gypsum • Epsom salt 7 December 2015 Sources of Sulfur Sulfur Mining of Sulfur Mining of Sulfur 7 December 2015 Sources of Sulfur Sulfur can be collected by two major process: 1. Sicilian Process 2. Frasch Process 7 December 2015 Frasch process In the Frasch process, three concentric tubes are introduced into the sulfur deposit. Superheated water (165 °C, 2.5-3 MPa) is injected into the deposit via the outermost tube. Sulfur (m.p. 115 °C) melts and flows into the middle tube. Water pressure alone is unable to force the sulfur into the surface due to the molten sulfur's greater density, so hot air is introduced via the innermost tube to froth the sulfur, making it less dense, and pushing it to the surface. The sulfur obtained can be very pure (99.7 - 99.8%). In this form, it is light yellow in color. If contaminated by organic compounds, it can be dark-colored; further purification is not economic, and usually unnecessary. Using this method, the United States produced 3.89 million tons of sulfur in 1989, and Mexico produced 1.02 million tons of sulfur in 1991. 7 December 2015 Frasch process 7 December 2015 Frasch process 7 December 2015 Sulfuric Acid History Islamic alchemists Jābir ibn Hayyān and Jamal Din al-Watwat included vitriol in their mineral classification lists. Ibn Sina focused on its medical uses and different varieties of vitriol. Sulfuric acid was called "oil of vitriol" by medieval European alchemists because it was prepared by roasting "green vitriol" (iron (II) sulfate) in an iron retort. Sulfuric acid (alternative spelling sulphuric acid) is a highly corrosive strong mineral acid with the molecular formula H2SO4. It is a pungent-ethereal, colorless to slightly yellow viscous liquid which is soluble in water at all concentrations. Sometimes, it is dyed dark brown during production to alert people to its hazards.The historical name of this acid is oil of vitriol. 7 December 2015 Sulfuric Acid Production Process 1. Contact Process 2. Chamber Process 7 December 2015 Sulfuric Acid 1. Contact Process The contact process is the current method of producing sulfuric acid in the high concentrations needed for industrial processes. Platinum was formerly employed as a catalyst for the reaction, but as it is susceptible to poisoning by arsenic impurities in the sulfur feedstock, vanadium(V) oxide (V2O5) is now preferred. This process was patented in 1831 by British vinegar merchant Peregrine Phillips.In addition to being a far more economical process for producing concentrated sulfuric acid than the previous lead chamber process, the contact process also produces sulfur trioxide and oleum. 7 December 2015 Sulfuric Acid 1. Contact Process The process can be divided into five stages: 1. combining of sulfur and oxygen 2. purifying sulfur dioxide in the purification unit; 3. adding excess of oxygen to sulfur dioxide in presence of catalyst vanadium pentoxide, with temperatures of 450 degrees Celsius and pressure of 1-2 atm.; 4. sulfur trioxide formed is added to sulfuric acid which gives rise to oleum (disulfuric acid); 5. the oleum then is added to water to form sulfuric acid which is very concentrated. 7 December 2015 Sulfuric Acid 1. Contact Process H2S407 7 December 2015 Sulfuric Acid-Reaction -1 Sulfur dioxide and oxygen then react as follows: 2 SO2(g) + O2(g) ⇌ 2 SO3(g) : ΔH = -197 kJ mol According to the Le Chatelier's principle, a lower temperature should be used to shift the chemical equilibrium towards the right, hence increasing the percentage yield. However too low of a temperature will lower the formation rate to an uneconomical level. Hence to increase the reaction rate, high temperatures (450 °C), medium pressures (1-2 atm), and vanadium(V) oxide (V2O5) are used to ensure a 96% conversion. Platinum would be a more effective catalyst, but it is very costly and easily poisoned.The catalyst only serves to increase the rate of reaction as it does not change the position of the thermodynamic equilibrium. The mechanism for the action of the catalyst comprises two steps: 5+ 5+ 2- 4+ 1. Oxidation of SO2 into SO3 by V : 2 SO2 + 4V + 2 O → 2 SO3 + 4V 4+ 5+ 4+ 5+ 2- 2. Oxidation of V back into V by oxygen (catalyst regeneration): 4 V + O2 → 4 V + 2 O 7 December 2015 Sulfuric Acid Condition for maximum yield of SO3 1. Purification of gas 2. Oxygen supply 3. Temperature (450˚C) 4. Condition of catalyst 5. Pressure (1.5-1.7 atm.) 7 December 2015 Sulfuric Acid 2. Chamber Process Sulfur dioxide is introduced with steam and oxides of nitrogen into large chambers lined with sheet lead where the gases are sprayed down with water and chamber acid. The sulfur dioxide and nitrogen dioxide dissolve and over a period of approximately 30 minutes the sulfur dioxide is oxidized to sulfuric acid. The presence of nitrogen dioxide is necessary for the reaction to proceed. The process is highly exothermic, and a major consideration of the design of the chambers was to provide a way to dissipate the heat formed in the reactions. 7 December 2015 Sulfuric Acid 2. Chamber Process 7 December 2015 Sulfuric Acid 2. Chamber Process 7 December 2015 Sulfuric Acid 2. Chamber Process (Chemistry) Sulfur dioxide is generated by burning elemental sulfur or by roasting pyritic ore in a current of air: S8 + 8 O2 → 8 SO2 4 FeS2 + 11 O2 → 2 Fe2O3 + 8 SO2 Nitrogen oxides are produced by decomposition of niter in the presence of sulfuric acid or hydrolysis of nitrosylsulfuric acid: 2 NaNO3 + H2SO4 → Na2SO4 + H2O + NO + NO2 + O2 2 NOHSO4 + H2O → 2 H2SO4 + NO + NO2 7 December 2015 Sulfuric Acid 2. Chamber Process In the reaction chambers, sulfur dioxide and nitrogen dioxide dissolve in the reaction liquor. Nitrogen dioxide is hydrated to produce nitrous acid which then oxidizes the sulfur dioxide to sulfuric acid and nitric oxide. The reactions are not well characterized but it is known that nitrosylsulfuric acid is an intermediate in at least one pathway. The major overall reactions are: 2 NO2 + H2O → HNO2 + HNO3 SO2 (aq) + HNO3 → NOHSO4 NOHSO4 + HNO2 → H2SO4 + NO2 + NO SO2 (aq) + 2 HNO2 → H2SO4 + 2 NO 7 December 2015 Sulfuric Acid 2. Chamber Process Nitric oxide escapes from the reaction liquor and is subsequently reoxidized by molecular oxygen to nitrogen dioxide. This is the overall rate determining step in the process: 2 NO + O2 → 2 NO2 Nitrogen oxides are absorbed and regenerated in the process, and thus serve as a catalyst for the overall reaction: 2 SO2 + 2 H2O + O2 → 2 H2SO4 7 December 2015 Sulfuric Acid Comparison between Chamber process & Contact process Chamber Process Contact Process Dilute acid is produced (65-70%) Conc. Acid is produced Impure acid is produced Pure acid is produced SO2 is not use fully SO2 is used fully Purification of SO2 is not so necessary Purification of SO2 is necessary Purification of acid is costly No need purification process Production process less costly Costly It is very critical to make conc. acid Conc. Acid is produced 7 December 2015 Sulfuric Acid Physical Properties : MP : 10°C BP : ~338 °C Density : 1.840 g/mL at 25 °C(lit.) Vapor density : <0.3 (25 °C, vs air) Vapor pressure : 1 mm Hg ( 146 °C) Storage temp. : Store at RT. Solubility : H2O: soluble Water Solubility : miscible Sensitive : Hygroscopic 7 December 2015 Sulfuric Acid Chemical Properties : 1. Reaction With Water 2. Reaction With Metals 3. Reaction With Salt 4. Reaction With Alkali 5. As oxidizing agent 6. Action of Heat 7 December 2015 Uses - Sulfuric Acid 1. Production of acid (HCl, HNO3, HF), Washing soda, salt, explosive, dying industry, petroleum purification industry etc. 2. Drying of wet gas 3. Medicine industry 4. Storage cells, plastic industry 5. As a reagent in laboratory. 7 December 2015 Uses - Sulfuric Acid 7 December 2015 Sulfuric Acid 7 December 2015 Oleum Oleum or fuming sulfuric acid, is a solution of various compositions of sulfur trioxide in sulfuric acid, or sometimes more specifically to disulfuric acid (also known as pyrosulfuric acid). Oleums can be described by the formula ySO3.H2O where y is the total molar sulfur trioxide content. The value of y can be varied, to include different oleums. They can also be described by the formula H2SO4.xSO3 where x is now defined as the molar free sulfur trioxide content. Oleum is generally assayed according to the free SO3 content by weight. It can also be expressed as a percentage of sulfuric acid strength Oleum is produced in the contact process, where sulfur is oxidized to sulfur trioxide which is subsequently dissolved in concentrated sulfuric acid. Sulfuric acid itself is regenerated by dilution of part of the oleum. Oleum is the term used to describe fuming sulfuric acids. Oleum is made in various strengths and consists of SO3 dissolved in 100% H2SO4. Thus, for example, 20% oleum contains 20% SO3 and 80% H2SO4 by weight.
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  • Deepak Nitrite Limitd

    Deepak Nitrite Limitd

    Deepak Nitrite Ltd Technical Data Sheet Nitrosylsulphuric acid (NSA) ( Domestic ) 1. Introduction Nitrosylsulfuric acid is the chemical compound with the formula NOHSO4. It is a colourless solid that is used industrially in the production of caprolactam. 1. Product: Nitrosylsulphuric acid (NSA) 2. CAS No: 7782-78-7 3. Molecular Formula: HNO5S 4. Molecular Weight: 127.08 2. Physical Properties: Physical state: viscous liquid Appearance: Clear yellow to green viscous liquid Melting Point : -10 °C Stability: Store in cool place. Keep container tightly closed in a dry and well-ventilated place. Containers which are opened must be carefully resealed and kept upright to prevent leakage. Handle and store under inert gas. Density 1.890 – 1.895 g/cm3 ( at 20 °C ) Boiling point :- Decomposes Solubility in water :- Decomposes Solubility :- Soluble in H2SO4 Effective Date : 21.11.2012 Page 1 of 4 Deepak Nitrite Ltd 3. Product Quality Specification: Sr Parameter Standard Grade Un coated Number 01 Physical Clear yellow to greenish viscous liquid Appearance 02 Nitrosylsulphuric 35.0 to 40.0 %w/w acid (NSA) 03 Acidity as H2SO4 54.0 %w/w Min. Our products are not meant for use as food or drug additives. 4. Packing Information: Sr. Grade Packing Secondary Packing Number 01 Liquor In Tanker DNL Can customize packing for different quantities. 5.PRODUCT USES Chemical Properties Yellowish viscous liquid Usage Nitrosylsulfuric acid is used for diazotisation, nitrosation, oxidation and oximation reactions. Product Data Sheet General Description Shipped in solution with sulfuric acid (solutions are usually 40% Nitrosylsulfuric acid and 54% sulfuric acid (Hawley)). Solution is a straw-colored oily liquid with a sharp odor.