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April 10, 1945. ? April 10, 1945. ?. c. ????lsoN 2,373,528 METHOD OF RECOWERING MAGNESIUM COMPOUNDS Filed Aug. 13, 1941 AORNEY Patented Apr. 10, 1945 2,373,528 UNITED STATES PATENT OFFICE METHOD of RECovERING MAGNESIUM. ??M???NDs Thomas C. Atchison, Princeton, N.J., assignor to Johns-Manville Corporation, New York, N.Y., a corporation of New York Application August 13, 1941, serial No. 406,577 5 Ciams. (CI. 23-67) This invention relates to magnesium carbonate wasted when pipe lines, boilers, etc., are stripped compositions of the type suitable for insulating of old magnesia insulating materials. Also, min purposes. It relates particularly to a method of erals, either calcined or uncalcined, containing recovering magnesium compounds from materials relatively large proportions of magnesia. Walues, previously wasted and utilizing the recovered ma such as serpentine, chrysotile, etc., but which are terials in the process of manufacturing magne difficult to carbonate, may be utilized as a Source. sium carbonate compositions in the conventional of raw material in the operation of my present process heretofore practiced. invention. Through the use of the carbonating Heat insulating materials containing basic procedure, as will be described in more detail magnesium carbonate are generally made by 0. below, the magnesia components in these prod forming an admixture of basic magnesium car ucts, some of which were previously considered bonate and asbestos fibres, the fibres being pres waste materials, may be readily recovered, and ent to impart binding characteristics and addi the resulting recovered magnesium compounds. tional strength to the product. The mixture of may be used in preparing new magnesium com the basic carbonate and fibres is placed in suit is pounds for various purposes. able molds shaped in accordance with the desired It is, therefore, an object of this invention to design of the final product, and thereafter the recover magnesium compounds formerly lost in molded product is subjected to a drying action. waste materials and sludge which will thus in . In forming the heat insulating material the pro crease the plant capacity for the production of portions of the fibre and the basic magnesium 20 magnesium carbonate products by about 20-25 carbonate are so proportioned that the final prod per cent. The plant capacity will be increased uct contains. about 85 per cent of basiç magne to this degree, since the volume of the materials sium carbonate. This product is generally re passing through the equipment need not be in ferred to in commerce as 85 per cent magnesia. creased in order to make the recovery of the In preparing the basic magnesium carbonate 25 magnesium compounds from the waste products, used in 85 per cent magnesia, a considerable pro ' effective. The recovered products are merely en portion of the magnesium compounds obtained as tered into the regular production cycle and the a result of following the conventional procedure concentration of the magnesium solutions may of manufacturing magnesium carbonate mate be increased without detrimental effects which rials... are lost in waste water and waste sludges. 30 were previously encountered prior to the utiliz It has been estimated that magnesium com -ation of the present invention. V pounds to the extent of 20-25 per cent of the It is also an object of this invention to recover magnesia values in the raw materials have been the magnesium compounds formerly lost in waste lost in the waste waters and sludge which have materials at a negligibly increased cost in oper always in the past been discarded. recover 35 ating expenses. The recovery operation may also ing the magnesia values from the w astewaters be applied to recover magnesia values from trim and sludge a considerable reduction in cost of mings, old magnesia insulation materials and dif the manufacturing operations will be obtained. ficultly carbonatable minerals. The necessary It is known that an aqueous suspension of cal- . equipment for carrying on the present process cium carbonate and magnesium carbonate, as, for 40 is not very expensive, and the increased overhead example, 80 per cent calcium carbonate and 20 expense as a result of the equipment and Operat per cent magnesium carbonate, could be treated ing costs will be very small as compared to the with a large excess of strong carbon dioxide gas value of the magnesium compounds now recove - to dissolve the magnesium carbonate forming a ered but previously lost. magnesium bicarbonate solution and leaving the 45 It is a further objec, of this invention to ma calcium carbonate undissolved, but no economi terially reduce the amount of steam required cal method has thus far been developed to apply for precipitating the magnesium bicarbonate so the above separation to plant operations. lutions, inasmuch as the concentration of the Large quantities of magnesium carbonates have magnesium bicarbonate solution can be materi also in the past been wasted in the form of trim 50 ally increased. Previously, it was undesirable to mings obtained during the sizing and finishing have too high concentrations of the magnesium operations of crude molded basic magnesium car bicarbonate solutions because of the fact that a ... bonate products. These trimmings are usually in substantial proportion of the magnesium com the form of a dust and small lumps. Additional pounds precipitated from the solution and were . quantities of magnesium compounds have been 55 thereby lost in the waste waters and sludge. 2 2,878,528 However, through the application of the present is converted into a water-soluble magnesium novel procedure more fully described herein, the bicarbonate and the calcium hydroxide is con resulting increase in decomposition of the mag verted into a substantially water-insoluble cal nesium bicarbonate solutions is no longer of any cium carbonate. significance, since the decomposed material is 5 The magnesium bicarbonate solution contain recovered. Thus, since the magnesium bicarbon ing the water-insoluble calcium carbonate is ate solutions may now be used at higher concen thereafter pumped to a settling tank wherein the trations, the amount of steam formerly required water-insoluble components are permitted to set for boiling magnesium bicarbonate solutions to tle to the bottom of the tank. A small percent precipitate the magnesium carbonate may be re 0. age of the magnesium bicarbonate solution has a duced. tendency to precipitate in the form of normal Additional objects and benefits of the present magnesium carbonate (MgCO3.3H2O) which will invention will be apparent to those skilled in the settle with the calcium carbonate components art from the more detailed description of the in the bottom of the tank. novel method hereinafter set forth. "?? The substantially clear and sludge-free mag Broadly stated, the present invention includes nesium bicarbonate solution is then pumped to the treatment of waste sludges and other diffi a precipitator and the Solution is subjected to a cultly carbonatable materials containing retained hêating operation. During the heating the mag or absorbed soluble magnesium carbonate and nesium bicarbonate will precipitate from the solu insoluble magnesium carbonate with carbon di f) () tion in the form of an insoluble magnesium car oxide gas to form water soluble magnesium comi benate which may be in the form of normal mag pounds. The Water-soluble magnesium com nesium carbonate or the basic magnesium car pounds are then separated from the water-insol bonate, and this reaction is accompanied by the uble compounds, and the resulting solution con evolution of considerable carbon dioxide. The taining the water-soluble magnesium compounds 5 precipitated magnesium carbonate is then placed is used in conjunction with fresh magnesium into a filter or other dewatering device to remove compounds in the regular manufacturing cycle. the major portion of water, and the magnesium The invention will be illustrated by a more carbonate slurry is thereafter placed into suit complete description in connection with the at able molds of any desired shape, followed, if nec tached drawing, which shows a flow sheet of the essary, by the application of pressure. If fibres preferred embodiment of the method for recov are added to the material, the fibres may be ering magnesium compounds from waste mate added after a substantial proportion of the water rials. The broken line portion of the flow sheet has been removed from the slurry, that is, after is the conventional method heretofore used in the slurry has been passed through the filter. manufacturing basic magnesium carbonate prod 5 The lime sludge obtained from the lime sludge ucts. The portion of the flow sheet in heavy thickener contains a substantial proportion of lines illustrates the procedure followed in my in precipitated magnesium carbonate, retained or vention in recovering the magnesium compounds absorbed magnesium bicarbonate solution, cal from the Waste materials. cium carbonate, and other compounds. The per In the drawing illustrating a conventional 4 centage of magnesia values in these sludge prod method of manufacturing basic magnesium çar lucts, previously wasted, is very high, and it is bonate, dolomite mineral (composed primarily of , advantageous to recover these magnesia values magnesium carbonate and calcium carbonate) in order to increase the plant capacity over nor and coke are fed to a kiln and subjected to rela mal operations. tively high temperatures to convert the mag The sludge obtained from the lime sludge thick nesium carbonate and the calcium carbonate to ener is mixed with additional water until the magnesium oxide and calcium oxide, respectively. mixture forms a comparatively thin slurry. It is During the calcining action, carbon dioxide gas preferable that the slurry be diluted with water is evolved as a result of the reduction of the to Such a degree that the concentration of the magnesium carbonate and calcium carbonate to 5 O magnesium carbonates is at least below 1.5 per the respective oxides.
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