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US3099524.Pdf 3,099,524 United States Patent 0 Patented July 30, 1963 1 2 aluminium and magnesium with a mixture of sodium 3,099,524 hydroxide and sodium canbonate in appropriate amounts. ANTAClD CGMPOSITIONS The aluminium and magnesium salts are preferably the Frederick Grossmith, Pinner, England, assignor to chlorides. Beecham Research Laboratories Limited, Breutford, A further method for preparing the compounds of the Middlesex, England present invention is to suspend a magnesium hydroxo Filed June 28, 1960, Ser. No. 39,245 Claims priority, application Great Britain July 2, 1959 aluminate of the type disclosed in by said co?pending 6 Claims. (Cl. 23—l4) application Serial No. 842,042, ?led September 24, 1959, in a liquor containing bicarbonate ions. A suitable This invention relates to improvements in antacid 10 liquor is a dilute solution of magnesium bicarbonate. compositions and is particularly concerned with new A still further method for preparing the magnesium chemical compounds which have been found to have bicarbonate hydroxoaluminates, which method minimises desirable antacid properties being eminently suitable for the formation of a basic magnesium carbonate impurity, medicinal use for the treatment of gastric hyperacidity. is to react a solution containing aluminium and mag In my co-pending application Serial No. 842,042, ?led 15 nesium salts in appropriate amounts with sodium hy September 24, 1959, now abandoned, I have disclosed droxide at a suitable rate of delivery. An addition of certain novel compounds which are formed by reacting ‘sodium bicarbonate is made at an appropriate stage and aluminium and magnesium salts with caustic allcalis, in a ?nal addition of mixed sodium hydroxide and sodium which the magnesium content, expressed as Mg(OI-I)2, bicarbonate is made to precipitate all the magnesium lies between the approximate limits 2.5% to 75% by 20 without allowing the pH to rise too high. weight of the substantially dry product and in which Yet a further method of preparing the magnesium bi the aluminium content, expressed as Al(OI-I)3, lies be carbonate hydroxoaluminates is to react a solution con tween the approximate limits 75% to 25%. These com taining aluminium and magnesium salts in appropriate pounds, which we have termed magnesium hydroxo amounts with a solution of sodium carbonate. The car aluminates, have exceptionally desirable properties as 25 Ibon dioxide evolved from the reaction of sodium car antacids. bonate with the aluminium salt gives rise to bicarbonate We have now found that in magnesium hydroxoalumi ions and prevents the pH from rising high enough for nates the complex hydroxoaluminate ion is readily pene the direct precipitation of basic magnesium carbonate. trated by bicarbonate ions which replace the hydroxo A proportion of the double compound groups and that novel compounds are formed having a 30 constant ratio of two atoms of aluminium to one bicar NaMgH(CO3) 2.4H2O bonate ion. Accordingly, the present invention provides new com pounds Which are magnesium carbonate hydroxoalumi may be formed. As with the magnesium hydroxoalumin 35 ates, an inclusion of ammonium chloride limits the pre nates having the general formula cipitation of magnesium carbonate and thereby restricts double compound formation. A suitable a?ter treatment, for example, boiling the slurry, breaks down the residual double compound and completes the reaction to form 40 magnesium carbonato hydroxoaluminates. where n is an integer from 1 to 5. Yet another method of preparing the magnesium car The complete series of novel compounds is as follows: bonato hydroxoaluminates is to react a slurry prepared from basic magnesium carbonate, preferably Light Mag nesium Carbonate B.P., and a solution of sodium car bonate with a solution of aluminium chloride. The re Molec action may be initiated in the cold and aiiter diluting to ular Mg A1 Mg(OH)2 Al(OH)a 002 a suspension containing approximately 5% solids w./v. Weight by boling for a period. The following examples illustrate the invention: Mg[A.lz(OH)7.HCO3]._ 258.35 9.42 20.58 22.58 60.38 17.04 Mg2lAl2(OH)a.HCOa]._ 316.69 15.36 17.04 36.84 49.26 13.90 50 Mg3[Al2(OH)11.HCOa]. 375.03 19.46 14.39 46.67 41.59 11.74 Mg4[Al2(OH)1a.HCO3L 433.36 22.45 12.46 53.83 36.01 10.16 Example 1 MEslAlAOHhs-ECOaL 491.70 24.72 10.98 59.29 31.76 8.95 A solution of sodium aluminate, Na3[Al(OH)6] was 55 prepared from 48.27 g. of AlCl3.6H2O and 64.00‘ g. of The lower members of the series of the new com NaOH by adding slowly a solution of the aluminium pounds may be prepared by reacting a cold solution of chloride in 500 mls. of water to a solution of the so magnesium bicarbonate or a cold solution of a mag dium hydroxide in 500 mls. of water at room temperature. nesium salt and sodium bicarbonate, with a cold solu The clear solution produced was added to 1,760 mls. tion of an alkali aluminate, e.g. sodium aluminate. The 60 of a 2.5% solution of magnesium bicarbonate contain higher members of the series cannot be prepared by this ing free carbon dioxide and in which the pH was ad method as the magnesium is partially precipitated as basic justed to 9 by the addition of sodium hydroxide. At this carbonate. point of addition of sodium hydroxide the solution was Alternatively, the compounds may be prepared by re just beginning to appear opIalescent. The addition of acting a solution of the appropriate amount of salts of 65 sodium al-uminate solution to magnesium bicarbonate solu 3,099,524 a . 4 tion was made at room temperature with constant stirring. added to a 5 litre beaker. The sodium hydroxide solu Finally, the precipitate was washed on a basket type tion was transferred to a dropping funnel and this solu centrifuge and was dried at 52° C. tion was introduced dropwise into the mixed chloride solution, which was agitated using a twin blade propeller Example 2 type stirrer, the mixing being carried out at room tem perature. During the addition of the sodium hydroxide The following solutions were prepared: a periodic check of pH was made and when the pH was approximately 7.0 the sodium bicarbonate solution added MgCl2.6H2O, 61 g. ___________ _. In water to give 500 to the mixture. A1Cl3.6H2O, 24.15 g. _________ .__ { mls. of solution. 10 At the completion of the addition of the sodium hy NaOH, 32 g. ________________ _- In water to give 500 droxide (after approximately 1 hour), 500 mls. of the Na2CO3, 10.6 g. _____________ __ { mls. of solution. sodium sesquicarbonate solution were added, when it was found that magnesium ion in the supernatant liquor The solutions were heated to 70° C. and then mixed was reduced to 100 ppm. The precipitate was then by pouring simultaneously into a 2 litre beaker. While washed with distilled water on a basket type centrifuge continuing to stir with a twin blade propeller type stir and was dried at 52° C. rer the slurrry was heated to 90° C. and incubated at this temperature for 20 minutes. The material was then Example 6 washed on a basket type centrifuge and dried at 52° C. 20 This material contained as impurity magnesium hydrate The following solutions were prepared: and/or basic magnesium carbonate which impurity was removed by digestion with a solution of ammonium chlo ride to give magnesium carbonato hydroxoaluminate. MgCl2.6HzO, 51.25 g __________ _. In distilled water to Formula I 11:5 (2a). give 150 mls. of solution. Example 3 AlCl3.6H2O, 21.38 g. _________ _- Do. NaOH, 26.96 g. ______________ _. In distilled water to The ‘following solutions were prepared: give 200 mls. of solution. MgCl2Q6H2O, 68.37 g. ________ __ [In water to give 500 NaHCO3, 141.4 g _____________ __ In distilled water to AlCl3.6H'2O, 59.73 g. _________ __ }_ mls. of solution. give 2 litres of so NaOI-I, 113.98 g ______________ _. lIIl water to give 500 lution. mls. of solution. 35 The solution of aluminium chloride was added slowly The solutions were heated to 90° C. then mixed by to the solution of sodium hydroxide, with vigorous stir adding the NaOH solution to the mixed chloride solution, ring. The sodium aluminate solution so prepared was over a period of 2 minutes. The mixture was incubated added to the mixed magnesium chloride solution and at 90° C. for 10 minutes. sodium bicarbonate solution, the mixing being carried The precipitate was Washed by decantation in a 5 40 out at room temperature, with constant stirring employ litre beaker, using as wash liquor 50 litres of approxi ing a twin blade propeller type stirrer. The precipitate mately 0.04% w./v. solution of magnesium bicarbonate was washed, employing a basket type centrifuge and was in distilled water. It was then ?ltered and washed on then dried at 52° C. the ?lter with distilled water, ?nally being dried at 52° C. A portion of approximately 6 g. of the precipitate was 45 suspended in 300 mls. of an approximately 2 volume Example 4 solution of carbon dioxide in water for 8 hours. After suspension in the carbonated water, the precipitate was The same quantities of reactants as those shown in Ex again washed and dried at 52° C. The molar ratio ample 3 were employed and the procedure followed was Mg:Al of the precipitate before suspending in carbonated similar, except that washing by decantation wasrcarried water was 1.7:1 and a pH peak of 7.4 was ‘found on the out using mains water containing 268 mg.
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