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Patented Oct. 30, 1928. 1,689,775 ‘UNITED STATES PATENT OFFICE.

WALLACE L. CHANDLER, OF EAST LANSING, MICHIGAN. GALCICATED AND PROCESS OF PREPARING SAME.

No Drawing. Application ?led May 1, 1924. Serial No. 710,420. This invention relates to an improved The total iodine content, in combination and calcicated iodine and the process of prepar in solution, is from .7 % to 1.2%. The ing the same. The material I call calcicated strength depends on the strength of the hy droxide used. The stronger is produced iodine. 60' 5 The main objects of the invention are: when there is a small amount of First, to provide an improved stable iodine hydroxide in suspension. This solution may compound or a composition or mixture of be slightly cloudy from the small amount compounds capable of disintegrating under in suspension, such slight cloudiness being the e?ects of weak acids to produce free permissible. Iodine in excess is required for 65 10 active iodine in solution at the points of a continuous process. application of medication, and-the process 1 The probable main reactions are as fol of roducing the same. ows: . > econd, to provide an improved stable calcicated iodine compound or a composition 70 15 or mixture of compounds in aqueous solu tion capable of yielding, under the e?ects of strong acids, the right concentrations and Thus, leaving out the intermediate ‘steps ' proportions of hydriodic acid and iodic which are quite transient, we have : acid in solution so that the latter will im 6C8. 2 + 6I2—>5C8.I2 + g + 75 20 mediately yield su?icient to vigor If the ?uid is allowed to remain in the con ously and completely oxidize all of the hy tainer, in the presence of iodine crystals, driodic acid in solution and that. formed as after the above reactions have been com- . the result of the disintegration of the iodic pleted, some iodine will go into solution in acid, precipitating a water-soluble crystal the salts formed; but this fact in no way 25 line form of iodine. This has the properties described in my copendin patent applica injures the chemical properties of the prod tion ?led March 16, 1923, éerlal No. 625,670. uct.My improved composition 'calcicated' ' io Objects pertaining to the details of the dine has the following pro erties: It is a process of preparation will de?nitely appear colorless, oderless (except t at at times it 30 from the description to follow. as I accomplish the objects as pointed out in has a faint “iodoform” oder) liquid with a the following s eci?cation. The invention slightly alkaline reaction and consists of is clearly de?ne in the claims. approximately ?ve parts of calcium' In carrying out my invention I place a and one part in solution. Upon acidi?cation'with a strong acid, such 3 GI quantity of sublimed iodine (an excess of that required for the reactions) into a‘glass, as sulfuric acid, a crystalline form of iodine earthware or wooden container, such for is precipitated. “ . ' instance as a wooden barrel, and then ?ll The object of treatin crystalline iodine the container with a saturated aqueous solu with‘ the clear, or at best ut slightly cloudy, solution of lime instead of with the milk of 95 40 tion of . The calcium hy droxide is obtained by treating “building lime or moistened lime, as are the ordinary lime” with a large quantity of water, allow practices in the preparation of “iodated 4, ing the undissolved particles to settle and lime”, is that, since ‘calcium iodate is but removing the clear su ernatant ?uid, by sparingly soluble in concentrated solutions 100 45 drawing it off or otherwise. The contents of of calcium iodide, in the ordinary processes the container are agitated‘ at intervals in the calcium iodide is so highly concentrated order to insure a complete reaction between that the/ calcium iodate ‘formed precipitates the calcium hydroxide and the iodine, until in the vform of hexahydrated ‘calcium iodate, the ?uid takes on a permanent red-wine and there does not remain in solution a su?i color. The agitation insures the-excess of cient amount of monohydrated calcium. 50 iodate to yield, on acidi?cation with a strong iodine. . This ?uid then consists of a mixture or acid, the required amount of oxygen to com composition of the compounds: calcium plete the reactions necessary to bring about iodide (?ve parts) and calcium iodate (one the precipitation of crystalline iodine; part) with iodine in solution in these salts. whereas by my improved process, the pro 2 1,689,775 portions of the iodide and the, iodate are 2. A calcicated iodine comprising a com-V exactly right to bring about, on acidi?ca position. containing iodine and a compound 20 tion with a strong acid, the liberation of all of calcium and iodine. of the iodine. - 3. A stable calcicated iodine, being a com The object of using a glass, earthenware or position containing an excess of iodine con wooden container is that most metals form sisting of a mixture of approximately ?ve with iodine which increases the parts of calcium iodide, one part of calcium 25 iodides above the iodates to such an extent iodate and an excess of iodine in solution. that no crystalline iodine is precipitated 4. The process of preparing calcicated 10 from the solutions when acidi?ed with a iodine consisting in introducing into a con strong acid. tainer a quantity of sublimed iodine‘, in ex Having thus described my invention, what cess of that required for reaction, adding 30 I claim as new and desire to secure by thereto a comparatively lar e volume of Letters Patent is: saturated aqueous solution 0 calcium hy 15 1. A stable aqueous solution of calcicated droxide, and agitating the mixture. iodine containing an excess of iodine capable In witness whereof, I have hereunto set of yielding, under the in?uence of a strong my hand. acid, a crystalline form of iodine. WALLACE L. CHANDLER.