Vanadous chloride preparation

REDUCTION WITH VANADOUS CHLORIDE Preparation of Vanadous Chloride 213]... 

Aqueous solutions of vanadous chloride (vanadium dichloride) are prepared by reduction of vanadium pentoxide with amalgamated zinc in hydrochloric acid [213], Reductions are carried out in solution in tetrahydrofuran at room temperature or under reflux. Vanadiiun dichloride reduces a-halo ketones to ketones [214], a-diketones to acyloins [215], quinones to hydroquinones [215], sulfoxides to sulfides [216] and azides to amines [217] (Procedure 40, p. 215). 

Potassium Vanadicyanide, K3[V(CN)6], is prepared by the addition of excess of concentrated potassium cyanide solution to a concentrated solution of vanadous chloride, VC18 precipitation in the cold with alcohol gives rise to small rhombohedral plates. The solution is not very stable and rapidly becomes turbid, while addition of an acid produces the green colour which is characteristic of the V ion. The complex ion [V(CN)8]" appears, therefore, to be unstable, unlike the corresponding [Fe(CN)e] ", [Cr(CN)J ", and [Co(CN)e] " complex ions. The solution reacts with salts of heavy metals to yield variously coloured precipitates of double cyanides.7... 

The vanadium pentoxide catalyst Is prepared as follows Suspend 5 g. of pure ammonium vanadate in 50 ml. of water and add slowly 7 5 ml. of pure concentrated hydrochloric acid. Allow the reddish-brown, semi-colloidal precipitate to settle (preferably overnight), decant the supernatant solution, and wash the precipitate several times by decantation. Finally, suspend the precipitate in 76 ml. of water and allow it to stand for 3 days. This treatment renders the precipitate granular and easy to 6lter. Filter the precipitate with suction, wash it several times with cold 5 p>er cent, sodium chloride solution to remove hydrochloric acid. Dry the product at 120° for 12 hours, grind it in a mortar to a fine powder, and heat again at 120° for 12 hours. The yield of catalyst is about 3 - 5 g. 

Phthalocyanine 2 can be prepared from 3-phenylphthalic acid (1) and vanadium(III) chloride in the presence of urea and ammonium vanadate at high temperature in a melt.401... 

Anthrapyrimidine and its substituted derivatives are obtained by condensation of 1-aminoanthraquinone (or its derivatives) with formamide or aqueous form-aldehyde/ammonia in the presence of an oxidant, such as ammonium vanadate or m-nitrobenzosulfonic acid. A newly developed, more simple route proceeds via formamidinium chloride, which is prepared from 1-aminoanthraquinone with di-methylformamide and thionyl chloride or phosphorus oxychloride. Cyclization in a solvent in the presence of ammonium acetate affords the desired product ... 

Preparation of Vanadium Oxychloride by Reacting Vanadium(V) Oxide with Thionyl Chloride. Place 16 g of ammonium vanadate into a porcelain crucible. Roast the substance up to a constant mass at 500-550 °C in a crucible furnace, passing oxygen into the latter via a glass tube from a gas meter. 

Barium Pyrovanadate, BaaVaO is precipitated on addition of barium chloride to a solution of sodium pyrovanadate or of other vanadates in the presence of ammonia.3 It has more recently been prepared by the action of barium peroxide on vanadium pentoxide.4 It is a white, amorphous powder which melts above 868° C.5... 

Cyanopyrazine is obtained in 90% yield by the reaction of phos-phoryl chloride and carboxamidopyrazine. The reactants are first kept at room temperature for 5 hours and then heated under reflux for 40 minutes.228 Commercially, cyanopyrazine is prepared by reaction of methylpyrazine with a mixture of ammonia and air in the presence of a catalyst. The catalysts used are Co, Fe, Sn, and Ag vanadates and vanadium phosphotungstate.229 Bromopyrazines are readily converted into cyanopyrazines by treatment with cuprous cyanide in boiling y-picoline.230... 

One of the simplest methods of preparation is by decomposition of a thermally unstable compound. The nitrate or chloride is often preferred, sulphates tend to decompose at higher temperatures. Where the presence of residual traces of anion is to be avoided, the metal salts of organic acids are particularly useful. Formates, oxalates, acetates etc, decompose at low temperatures and often reduce the metal at the same time. For the preparation of catalysts from anions, the ammonium salt is frequently used. Metallic salts of complex acids can be used as a source of metal oxide mixtures. Decomposition of the appropriate chromate, tungstate, molybdate or vanadate will produce the mixed oxide. 

Ultrasonic irradiation has been employed for the low temperature synthesis of nanoparticles, recently in conjunction with benzyl alcohol and metal chlorides. Nanoparticles of Ti02, WO3 and V2O5 have been prepared in this manner. In the case of the vanadate, an additional heating step at 450 °C is required for complete conversion. This fast procedure allows for the preparation of crystalline nanoparticles. 

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