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UNITED STATES PATENT OFFICE 2,483,469 BASIC LEAD PHOSPHITE PIGMENTS Leonard M

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UNITED STATES PATENT OFFICE 2,483,469 BASIC LEAD PHOSPHITE PIGMENTS Leonard M Patented Oct. 4, 1949 2,483,469 UNITED STATES PATENT OFFICE 2,483,469 BASIC LEAD PHOSPHITE PIGMENTS Leonard M. Kebrich, Brooklyn, N. Y., assignor to National Lead Company, New York, N. Y., a corporation of New Jersey No Drawing. Application February 14, ‘1947, Serial No. 728,721 4 Claims. (Cl. 106-297) 1 2 This invention relates to basic lead phosphite tion catalyst, namely lead acetate, to facilitate compositions useful as pigments and more par the reaction. ticularly to the preparation and use of dibasic When the dilute phosphorous acid is added to lead phosphite and combinations of this com the aqueous suspension which has a pH value of pound with monobasic lead phosphite. approximately 9.3, no change in the pH value Monobasic lead phosphite is known and has ‘occurs until, on the addition of sui?cient phos been previously prepared by prolonged digestion phorous acid the suspension turns white. At of normal lead phosphite with ammonium hy this point a lowering of the pH value to 6.9 takes droxide and by reacting a solution of basic lead place and the White solid phase is found to con acetate with ammonium phosphite. The prod 10 tain on analysis 90.17% PbO', 4.18% P and 2.43% ucts thus obtained by the prior art methods have m0, corresponding to the compound dibasic lead been identi?ed as monobasic phosphites and were phosphite, 2PbO.PbHPO3.1/2H2O. This com found to contain a maximum of 85.9% lead oxide pound is constituted of well de?ned acicular crys PbO, corresponding approximately to the formula tals which are anisotropic in character. Due to for monobasic lead phosphite hemi-hydrate, 15 the dif?culties of obtaining proper optical orien PbO.PbHPO3.l/2H2O. Other basic lead phos tation, the several indices of refraction were not phite compounds have not been described previ easily determined, but one of the refractive in ously, so far as is known. dices was found to be about 2.25. The tinting A principal object of this invention is to pro strength of this pigment was found to be un vide a White basic lead phosphite composition 20 usually high, approaching a value of 300 in com useful for pigment purposes containing more parison to 190 for Dutch process white lead, than 85.9% PbO. Another object of this inven when tested by the method described in “Exami tion is to provide a new chemical compound, di nation of Paints, varnishes, Lacquers and Colors,” basic lead phosphite, corresponding to the for by H. A. Gardner, 6th edition, p. 65, mula 2PbO.PbHPO3.l/2H2O. Another object of On further treatment with phosphorous acid, this invention is to provide basic lead phosphite the dibasic lead phosphite is converted to mono pigments characterized by high tinting strength basic lead phosphite, PbO.PbI—lIPOs.1/2I-I2O, dur and opacity. A further object is to provide sur ing which conversion the pH value of the sus face coating compositions containing basic lead pension remains constant at about 6.9. Thus, by phosphite having excellent opacity and covering maintaining the pI-I value of the suspension at power and further characterized by excellent re about 6.9, it is possible, by using calculated sistance to weathering. A still further object of amounts of materials, to produce mixtures of di this invention is to provide white rust inhibiting basic and monobasic lead phosphite. These pig surface coating compositions especially valuable _ ments are insoluble in water and desirable from for protection of metal surfaces against corro ’* the standpoint of their pigment properties. sion. These and other objects will be apparent For the purpose of being more clearly under from the following description of the invention. stood, the preparation of dibasic lead phosphite This invention in its broadest aspects contem and mixtures of the dibasic and monobasic lead plates the preparation of a new chemical com. phosphite will be illustrated by the following ex pound, dibasic lead phosphite, and also coalesced mixtures of this compound with monobasic lead amplesr: EXAMPLE I phosphite, in ?nely divided form, adapted for Dz‘basic lead phosphite use as a pigment. The primary product of this invention, dibasic lead phosphite, represented by 1200 grams of ?nely powdered litharge were the formula 2PbO.PbHPO3.1 / 21-120, is in the form ., suspended in 5 liters of water containing 1.2 of ?ne acicular crystals, is of good white color, grams of glacial acetic acid. The suspension was and possesses high tinting strength and covering heated to about 50° C. and vigorously agitated power. while 507.1 grams of a 29% phosphorous acid A general method for preparing dibasic lead solution was slowly added over a period of 5% phosphite is ?rst to prepare a ?nely powdered hours. The white solid obtained on ?ltration suspension of lead monoxide or litharge in warm was found on analysis to contain 89.9% lead water containing a small quantity of lead acetate oxide, 7.30% phosphorous trioxide and 2.8% com and then while agitating. slowly adding dilute bined water corresponding to the formula phosphorous acid, using amounts su?icient to pro 2PbO.P-bHPO3-1/2H20‘. duce the dibasic salt. It will be noted that the EXAMPLE II process of this invention differs from the proc Equz'moleculdr mixture of dfbasic and monobasz'c esses of the prior art in that lead oxide and phos lead phosphites phorous acid are the principal reactants and that the reaction is conducted in an aqueous me 223.2 grams of powdered litharge were sus dium in the presence of a small amount of a solu pended in 1100 ml. of water containing 0.22 grams 2,483,469 3 4 of glacial acetic acid. The suspension was heated proper drying after each coat. The panels were to about 50° C. and while stirring, 113.1 grams exposed to natural weather conditions on ver of a 29% phosphorous acid solution was gradu tical test fences with a southern exposure. After ally added over a 5% hour period. The white 33 months the relative ratings of the two paints, product after ‘being ?ltered and dried, was found with 10 the optimum, were as follows: to contain 88.4% lead oxide and 8.70% phos phorous trioxide and 2.9% combined water. Paint No ________________________________________________ __ 1 2 The methods described in the preceding ex amples are convenient for laboratory procedures. 8 9 A method more adapted to commercial practice, 7 l0 l0 9 however, is to mix the components in their proper l 3 proportions with water and to grind them to Cracking ________________________________________________ __ l0 8 gether in a ball mill or other conventional grind ing mill for several hours in which case a com It is thus evident that outside white paints plete reaction is effected at normal room tempera prepared from dibasic lead phosphite are ap ture. Such a procedure is illustrated by the ,fol proximately the equivalent, in respect to weath lowing example: ering, of those prepared from basic carbonate white lead which has long been recognized as the EXAMPLE III standard pigment for exterior paints. Dz'basic lead phosphite That dibasic lead phosphite is also suitable as A mixture consisting of 1200 grams litharge, a rust inhibiting or anti-corrosion paint as illus 507.1 grams of a 29% phosphorous acid solution, trated by the following: 1.2 grams of glacial acetic acid and 6 liters of EXAMPLE V water was placed in a 5 gallon porcelain lined ball The following paints were prepared in the mill with 14 lbs. of ?int pebbles. The mill was usual manner. sealed and rotated for several hours at room temperature. The reaction product, a suspen sion of ?ne acicular crystals, was transferred to a Paint N 0 ____________________________________________ _ _ 3 4 tray and dried at about 60° C. The dried product Dibasic lead phosphite _____________________ “pounds” 34.1 .... __ was found to be dibasic lead phosphite, compara Red Lead (98% grade)._ do_._. _____ _. 42. 4 Iron oxide _____________ ._ 6.9 ble to the product of Example 1. Magnesium silicate ...... _ _ l0. 3 Lead phosphite pigments prepared as outlined Gumarone-Indene coal tar 24. 9 above may be made into surface coating compo Coal tar naphtha ________________ __ l5. 5 sitions, such as paint, by ordinary well known methods. The physical and chemical properties, 35 These paints were equivalent in composition useful for compounding paint formulations, for on a volume basis when corrected for the volatile both dibasic and monobasic lead phosphite are thinner content. tabulated below. Compositions consisting of They were applied to hot-rolled steel panels, coalesced mixtures of the dibasic and monobasic both sides, two coats being employed. A cover salts will show properties dependent on the pro coat of a suitable anti-fouling paint was then portionate amount or‘ each present in the com applied. The panels were tested by immersion position. in marine waters. After 13 months immersion the two paints were examined. The results are noted below, where a rating of 10 indicates opti Dibasic Lead Phospliite M??gfjgigéead 45 mum resistance to the type of failure under question. Formula_..._____ 2PbO.PbHPO3.l/2H2O__ PbO.PbHP0:.l/2H2O. Percent PbO...“ . % 85.9% Speci?c gravity. 95 6.95. Paint No. 3 4 Crystal Habit" acicular Color..__.__.__.__ white. 50 Tinting strength. about 220. General appearance—blistering __________________________ __ 7 6 Oil absorption __ 17-..". _-_ l5. Peeling from metal base _____________ _ . 9 7 Solubility in Insoluble .............. ._ Insoluble.
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