T h e story of zirconium chemistry in industry starts in the molten rocks of the earth, for the evidence of the behavior of the zirconium atom in the rocks presages the behaviors encountered in the preparation and isolation of the element or its useful compounds. Zirconium is moderately abundant in magmas and the rocks derived from magmas, its concentration in the crust of the earth being roughly equal to that of carbon, i.e., about 0.0270. As siliceous magmas cool, one of the first phases to crystallize is zircon, Zr02.SiOz. Its formation is favored by a moderate excess of acidic oxides in the magma, and i t is particularly likely to crystallize from magmas which yield granites and syenites. Once the zircon has formed, it is extremely stable, and much of the zircon that has formed in nature has survived hundreds of millions of years of geologic change, through upheavals, weathering, and changes in physical and chemical environment. The tetrrh-dral crystals are easily recognized.Even in ancient times, well-formed colorless and colored zircon crystals which had been freed from the matric-s in which they had developed found their way into the arts and ornamentation. Mention is made of the zircon in both Old and New Testaments
solvent is facilitated by vigorous stirring and by the installation of a hot plate several inches from the flask. The hot plate is removed before the sulfur dioxide is completely evaporated. The crystalline product is broken up with a glass spatula before it freezes to a hard cake, and the flask is placed in a vacuum desiccator over sulfuric acid. The desiccator is evacuated to remove the remaining sulfpr dioxide. Thirty-eight grams (96% yield) of crude sulfonic acid are obtained, melting at 57-59°C. The crude product is dissolved in 150 cc. of water and the diphenylsulfone removed by filtration. The solution is treated with activated charcoal to remove color and then concentrated under reduced pressure on a steam bath. After boiling has completely stopped, the flask is cooled. Thirty-five grams (79.5% yield) of crystalline product (benzenesulfonic acid monohydrate) are obtained, melting at 46-49°C. This material may be distilled from a 100-cc. distilling flask (all-glass apparatus) under reduced pressure. No attempt is made to distill the liquid until it is completely degassed. Water appears as condensate in the dry ice trap. After degassing at about 1 mm., the product is distilled at a pressure of less than 1 mm. maintained by a Cenco-Hyvac pump. A forerun of about 2 grams is collected, and then the main product distills at 130°at less than 1 mm. Twenty-two grams (56% yield) of pure white benzenesulfonic acid are collected, melting at 60-61°C. There is no apparent gassing during distillation. The residue is all water soluble. PREPARATION OF SODIUM BENZENESULFONATECrude benzenesulfonic acid prepared as described is dissolved in 150 cc. of water. The aqueous solution is boiled to remove sulfur dioxide. After treatment with activated charcoal to remove color, the aqueous solution is filtered, neutralized with 15 grams (0.121 mole), the theoretical amount, of sodium carbonate monohydrate. The solution is concentrated on a steam bath under reduced pressure until crystallization begins. The mixture is cooled to 0°C. and filtered. The mother liquor is treated again in the same manner.The combined product is dried in an oven at 105°C. to produce 31 grams (69% yield) of pure white sodium benzenesulfonate. Evaporation of the neutral solution to dryness will give 35.5 grams (79% yield) of sodium benzenesulfonate with an off-white color. CONCLUSIONS 1. It is possible to prepare aromatic sulfonic acids and their
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