Document X7xdrJbmd5dEe3KMG2ENowmOg

E. L DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Serial No.^ K1I-51-24 Copy Ho. 1. Numerical File NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report (Laboratory) EXTRACTION OF "VANADATE SLUDGE" Period Covered FEBRUARY 1051 TO MARCH 1951 FILE: DATE: ae&Tr 4-50-51 NJ 9747 Serial so# KH-51-24 copy m* 1 Humerlcal File ,Copy to * #1 Hnmerleal Pile 9 * Retearoh 0mo <223.21 $ - Ufcrary File {2S5i 4 - 1* Arnold Plant Filet . 8 * W. F. Spengemaa/J* S* Callaway/?. I - W. S* StaPWe/P7 J. Monahan 7 - J. H. Tully/A. Siegel/Library Monahan NEWARK PLART PIGMEST COLOR RESEARCH REPORT Final Report (Laboratory) EXTRACTION OP aVAHADATE SLUDGE* PEBROARI, 1951 to MARCH, 1951 Charge* 11(00}-11*24 (A-I-24) 4-30-51 DUP050068508 ISTROPHCTIOSt impsnding shortage of tungsten and molybdenum has led to an investigation of substitutes and their sources. TT. 3* Patent 2,195,258, assigned to the Du Pent Go*, describes color lakes made dim vanadates need aa all or part of the precipitant for basis dyes. EdgeMoor pivot has a sludge, conslstinglargely of fi0&, with a fairly high vanadium content. An investigation was trader* taken to determine the feasibility of recovering the vanadium at a cost which would make possible the manufacture of vanadate lakes. mjammimu 1. Vanadium can be recovered from the "Vanadate Sludge" by extraction with caustic soda. 2, Present Newark equipment does not lend itself to tho extraction, beoause of the large volumes of sludgo whim must be discarded. 3# A large amount of work appears necessary before phospho* vanadate lekes of acceptable quality earn be produced# mmmj work on the original sample of sludge showed that vanadium' could be extracted by an adaptation of tho sodium molybdate process, by boiling- with NaOH. From further work with a larger sample It mis learned that 8$, 10$ and 20$ HaOH solutions at the start off extraction (boiling was dons with open steam) ere squally effective In extracting vanadium# fern percent HaOH was Chosen for subsequent work beoause the slurry in a 20$ HaOH extraction was too thick, and the product from a 5% HaOH extraction was too dilute, HaOH must be used on the basis of the equation Vg06 + 6 HaOH ** 2 HagVO* SHgO, using about 20$ excess HaOH. Smaller quantities of HaOH, regardless of oeneom* tration, extract loss vanadium. It was decided that the extraction mas unattractive beoause of the large press volume required to handle the residual s&udgo, and because of an casing of the raw material supply situation for the normal prcoipltants for basis dyes# fhe extracted vanadate solution was evaluated in B2-264**:D (silioo-molybciat lake of "ViotorU Pure Blue BO") and in ABP*651*D (sllioo-molvbdate 1she of "Rhodamlne $ GKO, by substituting HaVOx (or its equivalent) ffr HajjHoOa, mol for mol# vanadium was supplied as (a), HH4VOs , D*6293, and (b>, as the extracted vanadate solution* The "Victoria Pure Blue BO* lakes were light, dull# very week, and poor in lightfastness. The lake from oxtraoted sludge was poorer than that fro HB4VO5. DUP050068509 m2 Tim first eilico-vanadate solutions for the "Rhodaminc* Isles precipitated before tbe strike* end tbe strikes sere discarded* Substitution of BoSO* for HC1 delayed* but did not present precipi tation in a second trial. Tbe strikes sere finished, and the resulting pigments sere dark and serf seek versus 1374-20-B* the reference standard. Xn an attempt to find tbs cause of tbs precipitation of the silico-vanadat solution* a number of SVA*a sere made* sitb different amounts of nineral acid* It sas Observed that fast acid addition gave faster precipitation* With sloe addition of H2SO4, tbe precipi tation sas progressively delayed as the quantity of acid decreased. ire phospho-varadate lakes sere attempted# DISOUSSIOHi Obviously* if silie0-vanadate or phospbo-vanadate lakes arc to be manufactured, formulation must be studied* There is no assur ance that vanadate nay bo substituted successfully, aol for vol. for tunstate or molybdate. Indeed, there are literature reference to indicate that it should not be so sthstituted* (See Bftckcl* "Structural Chemistry of Inorganic Compounds* p. 17 et s*q*) For future reference* the following phoapho-vanadie acids and salts art listed| 3 KgO.sPgOg . SVgOg.aq. 10 SrO.PgOg . SVgOg.aq. 4 (S%3g0 * %Og * SiVgOg.aq. 8 <H%)gO * SPgOg . eCVgOg.aq. 11 KgO * PfeOg . 24VgOg **q. 10 KgO * PSO5 . 24VgO *aq* 10 BaO * Pg05 * B4VB05 *aq* ` It will be seen that there is no * aoid oar- responding to the SHg0.Po0fi*24W0j r used as a basis for formulating phospho-tuastate lakes. letters* January through March, 1951* Chemical Division File Classification 121*1* on "Vanadium Sludge". Steel* "Structural Chemistry of Inorganic Compounds"* section on heter0-poly aolda* OJCKilg DUP050068510