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United States Patent Office Patented Nov 3,066,056 United States Patent Office Patented Nov. 27, 1962 2 both additives to synergistically provide the dihydrate 3,066,056 with enhanced stability against dehydration upon storage STABILIZED DICALCUM PHOSPHATE at about 60° C. at a relative humidity of about 75%. DHYDRATE Julian R. Schlaeger, Chicago Heights, and Lowel E. Similarly, Example IV, infra, shows that this combination Netiherton, Park Forest, E., assignors to Victor Chein 5 of constituents synergistically causes the dicalcium phos ical Works, Chicago, A., a corporation of inois phate dihydrate to have enhanced stability against dehy. No Drawing. Fied June 30, 1959, Ser. No. 823,822 dration in a glycerin-water solution. Example V, infra, 3 Claims. (C. 23-108) illustrates the control of the viscosity of toothpaste over a rather wide range with dicalcium phosphate dihydrate This invention relates to stabilized dicalcium phosphate O constituents which include in-process added pyrophos dihydrate compositions containing controlled proportions phoric acid and mechanically added calcium-sodium pyro of in situ formed calcium pyrophosphate and added phosphate in the same proportions that control the sta sodium-calcium pyrophosphate, dentifrice compositions bility of the dicalcium phosphate dihydrate against de containing said stabilized dicalcium phosphate dihydrate hydration. Example VI, infra, illustrates the procedure compositions, and methods of producing same. 5 that may be used for producing our stabilized dicalcium Dicalcium phosphate dihydrate is a highly desirable phosphate dihydrate. abrasive component for use in dentifrice formulations Determinations of stability of the dihydrate against because of its mild abrasive characteristics with respect to dehydration may be made by placing 10 grams of the tooth enamel. However, because of its instability against dicalcium phosphate dihydrate product (modified or un dehydration it is not entirely satisfactory for use in many 20 modified) in a 2/2-inch diameter moisture pan and hold dentifrice compositions. Partial or complete dehydration ing the pan in a humidor in an atmosphere of 75% rela of the dicalcium phosphate dihydrate in either powdered tive humidity and at a temperature of about 60° C. for or paste type dentifrice formulations results in undesirable periods ranging from 1 to 13 days. The amount of de variations in the abrasion and other physical characteris hydration may be obtained by determining the loss on tics of these formulations. For example, when used in 25 ignition after drying in a calcium chloride containing dentifrice paste formulations containing water and a desiccator for 1 to 2 hours at room temperature. By humectant such as glycerine or sorbitol, there is a tend comparison with an original sample, the difference in ency for the dicalcium phosphate dihydrate to become loss may be calculated as percent conversion to the an partially dehydrated on aging thereby causing the paste to hydrous salt. The stability data of Examples I-III, infra, become gritty or stiffen, or even set to form a hard non were obtained in this manner. extrudable mass. Considerable effort has been made in the past to EXAMPLE I stabilize the dicalcium phosphate dihydrate for use in In order to prepare dicalcium phosphate dihydrate, a dentifrice formulations. However, these efforts have met Weighed quantity of orthophosphoric acid may be diluted with only limited success, particularly in its use in paste with sufficient water to adjust the solution to about 15 type formulations such as the currently popular paste Bé. Strength. To this solution, a milk of lime slurry of formulations which include such gums as carboxymethyl about 8-10 Bé. strength may be added with rapid stirring cellulose and additives (e.g., sarcosinates, etc.) which at a rate sufficient to maintain the charge at a tempera provide these formulations with increased hygienic ture within the range of about 35 to 45° C. The addi properties. tion of milk of lime should be continued so as to com We have now found that the above difficulties may be plete the neutralization and precipitation of dicalcium substantially overcome by the combined use of controlled phosphate dihydrate crystals and produce a mother liquor levels of in situ formed calcium pyrophosphate and finely having a pH of about 7. The dicalcium phosphate di divided calcium-sodium pyrophosphate additives in con hydrate product may then be filtered-out and dried to junction with dicalcium phosphate dihydrate. This com 45 produce a product having particles smaller than about 40 bination of additives renders the dicalcium phosphate microns in diameter. dihydrate stable against dehydration under normal stor One percent by weight of finely divided sodium-calcium age conditions, gives it the ability to provide a suitable pyrophosphate (Cana2PO4H2O) should be mechani viscosity to toothpastes employing various humectants cally mixed with dicalcium phosphate dihydrate that was (e.g., glycerine and/or sorbitol), and stabilizes paste type 50 produced in accordance with the above-described proce dentifrice formulations containing dicalcium phosphate dure. This product is unstable because about 66% by dihydrate against changes which occur upon aging (e.g., Weight of the dicalcium phosphate dihydrate converted to changes in viscosity and gel strength). anhydrous dicalcium phosphate upon storage for one day It has been found that control of these characteristics at 60° C. in an atmosphere of about 75% relative hu may be effected by the introduction of from about 0.4% 55 midity. (or at least 0.16% HAPO) to about 0.8% by weight EXAMPLE II (based on the weight of the final stabilized dihydrate) As pointed out in Example I, above, dicalcium phos of pyrophosphoric acid (at least 40% H.P.O) in the phate dihydrate may be prepared by first diluting a process of manufacturing the dicalcium phosphate di Weighed quantity of orthophosphoric acid with sufficient hydrate plus the addition of about 0.6% to about 1.2% 60 water to adjust the solution to about 15 Bé. strength. by weight (based on the weight of the final stabilized di To this solution a milk of lime slurry of about 10 Bé. hydrate) of previously prepared, finely divided sodium strength may be added with rapid stirring at a rate suf calcium pyrophosphate to the finished, finely divided, ficient to maintain the charge at a temperature within the pyrophosphoric acid modified dicalcium phosphate di range of 35 to 45° C. The reaction may be permitted hydrate crystals. Both additions are essential to our in 65 to continue until the pH value of the liquor is about 5-6. vention since neither of these treatments alone produce At this point, 0.4% by weight pyrophosphoric acid should a dicalcium phosphate dihydrate composition having the be added to the reaction mixture. The addition of the above desired characteristics. milk of lime should be continued to complete the neu . Examples I-III, infra, show that the controlled addi tralization and precipitation of the dicalcium phosphate tion of both pyrophosphoric acid and sodium-calcium 70 dihydrate crystals and produce a mother liquor having a pyrophosphate to dicalcium phosphate dihydrate causes pH of about 7. The pyrophosphoric acid modified dical 3,088,056 3 4. cium phosphate dihydrate may then be filtered-out and EXAMPLE V dried to produce a product having particles smaller than about 40 microns in diameter. The product is unstable In order to illustrate the effect of our combination of as evidenced by the conversion of 44% by weight of the additives upon the viscosity of toothpastes containing di dicalcium phosphate dihydrate to anhydrous dicalcium calcium phosphate dihydrate, sorbitol and carboxymethyl phosphate upon storage for six days at the test conditions cellulose, viscosity studies were made with Formula Set forth in Example I, supra. tion-A, infra. Paste Formulation-A EXAMPLE III Percent by weight On the other hand, when the same levels of sodium calcium pyrophosphate and pyrophosphoric acid of Ex O Dicalcium phosphate dihydrate constituent (i.e., amples I and II, respectively, are both added in accord modified or unmodified dihydrate) ----------- 46.3 ance with the procedures set forth in these examples, the Sorbitol ----------------------------------- 25.0 resulting product is significantly more stable than the prod Carboxymethyl cellulose (as gum) ------------- 1.0 ucts produced by Examples I and II. Only 5% by weight Flavoring agents ---------------------------- O of the dicalcium phosphate dihydrate converted to the an Water ------------------------------------ 24.8 hydrous form upon storage for 10 days at the test condi Sodium lauryl sulfate ------------------------ 1.8 tions set forth in Example I, supra. Saccharin --------------------------------- 0.1 Example IV, infra, shows that the product of Example The viscosity measurements were made using a III, Supra, in glycerin-water solutions, is superior to the Brookfield Synchro-Lectric Viscometer (Multi-Speed products of Examples I and II, supra. Model. HAF). Each reported measurement represents the average of five separate measurements. The vis EXAMPLE IV cosity readings were converted to centipoises to give the Stability determinations of the dicalcium phosphate di values reported. hydrate in glycerin-water solutions were made by placing 2 5 It was found that the viscosities of pastes of the above 25 grams of the dicalcium phosphate dihydrate sample in type may be essentially controlled by controlling the pro a 100 ml. glass beaker and adding increments
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