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United States Patent (19) 11) 4,021,322 Dolan 45 May 3, 1977

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United States Patent (19) 11) 4,021,322 Dolan 45 May 3, 1977 United States Patent (19) 11) 4,021,322 Dolan 45 May 3, 1977 (54) ELECTROLYTIC PREPARATION OF 3,437,439 4/1969 Carroll ................................ 23/165 PHOSPHORUS ACID FROM ELEMENTAL 3,437,440 4/1969 Carroll ................................ 231165 3,528,772 9/1970 Whyte et al. ........................ 231165 PHOSPHORUs 3,532,461 10/1970 Whyte et al. ........................ 23/165 (75) Inventor: Michael J. Dolan, Manchester, Mo. OTHER PUBLICATIONS 73) Assignee: Monsanto Company, St. Louis, Mo. Inorganic Syntheses, vol. IV, 1953, pp.55-58, “Phos (22 Filed: Dec. 15, 1975 phorus Acid." (21) Appl. No.: 640,506 Primary Examiner-R. L. Andrews Attorney, Agent, or Firm-Wendell W. Brooks; John D. 52 U.S. Cl. ............................................... 204/103 Upham (51 Int. Cl'........................................... C25B 1122 (58) Field of Search .................................... 204/103 57 ABSTRACT (56) References Cited Elemental phosphorus is oxidized via indirect electro UNITED STATES PATENTS lytic oxidation to yield phosphorous acid, (HO),HPO. 3.437438 4/1969 Carroll ................................ 231165 12 Claims, 2 Drawing Figures OVERFLOW HX / H2O EVAPORATOR CRUDE HO)a HPO 14 CRYSTALLIZER (HO)2 HPO FILTER CRYSTALS ( Ho), HPo Li QUOR U.S. Patent May 3, 1977 4,021,322 <<<<<) SNSS arr an NNar NNN a C2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2:2 FIG... l. OVERFLOW HX / H2O EVA PORATOR CRUDE (Ho). HPo CRYSTALLIZER (HO)2 HPO FILTER CRYSTALS (HO)2 HPO LIQUOR 4,021,322 1 2 pared by the indirect electrolytic oxidation of elemen ELECTROLYTIC PRE PARATION OF tal phosphorus. PHOSPHORUS ACID FROM ELEMENTAL PHOSPHORUS DETALED DESCRIPTION OF THE INVENTION 5 The indirect electrolytic oxidation of elemental phos BACKGROUND OF THE INVENTION phorous to phosphorous acid conveniently represented This invention relates to the indirect electrolytic by reactions (2) through (5). oxidation of elemental phosphorus to phosphorous acid, (HO)HPO. ANODE REACTION 3 X -> 1% X + 3e (2) Phosphorous acid is available commercially as 30 10 percent and 70 percent aqueous solutions. The conven SOLUTION REACTIONS 1% X, + AP - PX (3) tional method of preparation of phosphorous acid com PX-3HO - (HO), HPO +3H +3X (4) prises hydrolyzing phosphorus trichloride according to the diagrammatically simplified reaction: CATHODE REACTION 3H + 3e - 1% H, (5) 15 PC-3HO - (HO)HPO +3HC (1) The net effect of reactions (2) through (5) of the present process are summarized as shown in reaction and evaporating the excess water and the hydrogen (6). chloride which are formed. However, the methods AP +3HO - (HO),HPO - 1% H. (6) involving these raw materials suffer from a number of 20 While not desiring to be bound by the theory of the disadvantages, most of which are inherent in the prior present invention, it is believed that the process com art methods. prises: One of the more obvious and vexing difficulties asso a generation of molecular halogen from the corre ciated with the known methods of preparation of phos sponding halide ion by electrolytic oxidation at the phorous acid is the absence of simple, effective, and 25 anode of an aqueous solution of hydrogen halide; efficient means of disposal for the large volume of b. oxidative reaction of the molecular halogen pro hydrogen halide produced during the conversion (ei duced during the electrolysis with elemental phos ther hydrolysis or otherwise) of phosphorus trihalide to phorus to form phosphorus trihalide, and the desired acid. Means which have been proposed for c. hydrolysis of the thus-formed phosphorus trihalide this purpose are generally expensive and less than satis 30 to produce phosphorous acid and halide. factory. Electrolytic reduction of hydrogen ions (protons) at As a result of the difficulties and disadvantages asso the cathode completes the electrochemical reaction. ciated with the known methods of preparation, phos Elemental phosphorus is a non-metallic element that phorus acid remains a relatively expensive chemical 35 exists in several allotropic forms (white or yellow, red, compound. and black or violet). All of these forms can be used in It has now been discovered that the difficulties and the present invention but the white or yellow (the terms disadvantages of the prior art methods are overcome by are used interchangeably) and red forms are preferred. the process of the present invention which represents a Of these, the white or yellow form is particularly pre substantial improvement in the sense that: 40 ferred. The term "elemental phosphorus,' as used a. the hydrogen halide generated is disposed of in situ herein, designates these allotropic forms. in a manner which facilitates it being recycled for White phosphorus exists as P, having a tetrahedral continued use with the result that only catalytic molecular structure. It is a brittle, waxy solid which has amount of hydrogen halide is required to be added a melting point of 44.1 C and a boiling point of 280.5 initially; and 45 C. Its vapor density corresponds to a formula of P. It is b. phosphorous acid is obtained relatively inexpen virtually insoluble in water and alcohol, moderately sively with a possible resulting decrease in the com soluble in chloroform, hexane, and benzene, and very mercial price of this important chemical com soluble in carbon disulfide. pound. Because elemental phosphorous is insoluble in water, A further advantage of the present invention is the 50 coupled with the fact that in the practice of the present ready availability of the essential reactants. The essen invention the electrolysis medium comprises elemental tial reactants are elemental phosphorus, hydrogen ha phosphorus and an aqueous solution of hydrogen ha lide (which is reusable), water, and electric current. lide, the elemental phosphorus is conveniently sus Various other advantages of this invention will be pended in the aqueous solution of hydrogen halide. come apparent from the accompanying description and 55 And further, since white phosphorus, the preferred claims. allotropic form, melts at 44.1 C, the electrolysis is conveniently carried out with the elemental phospho BRIEF DESCRIPTION OF THE DRAWINGS rus existing as a molten suspension. FIG. 1 is a schematic diagram of a cross section of an Thus, it is preferred to agitate the electrolysis me undivided electrolysis cell suitable for batch operation 60 dium vigorously so as to insure a relatively uniform of the present invention. dispersion of the elemental phosphorus throughout the FIG. 2 is a schematic illustration of a typical flow aqueous solution of hydrogen halide. Such agitation diagram of a process suitable for continuous operation also facilitates the dispersal of impurities and thereby of the present invention. minimizes the tendency of such impurities gradually to 65 coat the surface of the elemental phosphorus and pre SUMMARY OF THE INVENTION vent further reaction, particularly at process tempera According to the present invention, it has been dis tures in excess of its melting point. Still further, such covered that phosphorous acid is conveniently pre agitation insures thorough mixing the elemental phos 4,021,322 3 4 phorus and the molecular halogen produced during the The de Nora-type dimensionally stable anodes em electrolysis. Moreover, the preferred vigorous agitation ploy precious metal oxides plated on a titanium sub of the reaction mixture facilitates relatively rapid hy strate. Other materials include, for example, ruthenium drolysis of the phosphorus trihalide to phosphorous oxide, mixed with oxides of titanium and tantalum, also acid. The agitation can be carried out in any conven plated on a titanium substrate. Dimensionally stable tional manner such as by flow mixers, jet mixers, injec anodes suitable for use in the present process are cur tors, turbulence mixers, circulatory mixer systems, rently commercially available from the Diamond centrifugal pumps, and the like; by paddle and propel Shamrock Company, Cleveland, Ohio. ler mixers of various designs as well as by turbine or The anode materials of choice, by analogy with the centrifugal impeller mixers, colloid mills, and homoge 10 electrolysis of hydrochloric acid in chlorine cells which nizers. involves oxidation of chloride ion at the anode and The concentration of the aqueous solution of hydro reduction of hydrogen ions at the cathode, are graphite gen halide can vary widely, for example, from about 0.5 and de Nora-type dimensionally stable anodes. Graph percent to about 50 percent or more by weight of the ite functions in the present invention satisfactorily ex aqueous phase, but preferred concentrations will often 15 cept when an aqueous solution of hydrogen chloride is be in the range of about 1.0 percent to about 10 per employed as the source of molecular halogen. In such cent by weight, or on a molar basis, often in the range instances the electrolysis causes significant anode cor of about 0.1 molar to about 3.0 molar. It is to be noted, rosion to occur. It, therefore, becomes advantageous to however, that the concentration of the aqueous solu employ the de Nora-type anodes which are sufficiently tion of hydrogen halide has little effect on the current 20 stable under the reaction conditions utilized so as to efficiencies and product distribution (although there eliminate any corrosion problems. A further advantage might be a lower limit which would depend on the resulting from the use of dimensionally stable anodes is current density employed). the lowering of the halogen overvoltage with a concur Various current densities can be employed in the rent lowering of energy requirements. present process. It will be desirable to employ high 25 Any suitable electrode material may be employed as current densities in order to achieve high use of elec the cathode so long as it is relatively inert under the trolysis cell capacity which will result in increased pay reaction conditions and does not promote the produc load.
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