Perchlorates preparation

The perchlorate, prepared from neodymium oxide and perchloric acid [1] was purified and isolated as the salt tetrasolvated with acetonitrile [2], which has not been found to be shock-sensitive. On vacuum drying at 80°C/24h, it is converted to the disolvated salt which is very shock-sensitive and a 1 g sample exploded violently in a hand-held flask [3], Other examples of partially desolvated perchlorate salts becoming friction- and shock-sensitive are known [4], (The disolvate is very close to zero oxygen balance). 

Methyl, ethyl and propyl perchlorates, readily formed from the alcohol and anhydrous perchloric acid, are highly explosive oils, sensitive to shock, heat and friction [1], Many of the explosions which have occurred on contact of hydrox-ylic compounds with cone, perchloric acid or anhydrous metal perchlorates are attributable to the formation and decomposition of perchlorate esters [2,3,4], Safe procedures for preparation of solutions of 14 sec-alkyl perchlorates are described. Heated evaporation of solvent caused explosions in all cases [5], l-Chloro-2-propyl, iram-2-chlorocyclohexyl, l-chloro-2-propyl, 1,6-hexanediyl, hexyl, and 2-propyl perchlorates, prepared by a new method, are all explosive oils [6],... 

Xenon(Il) Fluoride Perchlorate. Preparation.—Perchloric acid (0.294 g, 2.93 mmol) was condensed into a Kel-F reactor containing XeF2 (0.477 g, 2.82 mmol) and was allowed to warm first to —110° and after 10 min to —60°. The reaction was... 

Benzyl-3-dimethylaminoallylidene- dimethylainmonium perchlorate prepared in analogy to (7 b-d) by formylation of benzylmalonic acid with DMF-POCI3 mp. 145° (92%)18 ... 

M lead perchlorate prepared by dissolving 9.20 g of Pb(C104)2.3H20 dried over a powerful dessicant for 60 hoiu"S and kept over this dessicant. 

All cations were used in the form of perchlorates. Preparation and purification of copper perchlorate have been reported (10). 

Some perhalates are especially strong oxidizing agents. Ammonium perchlorate, prepared from sodium perchlorate, is the oxidizing agent for the aluminum powder in the solid-fuel booster rocket of the space shuttle each launch uses more than 700 tons of NH4CIO4 ... 

Analogously, bis(i -l,2-diaminopropane)nickel(II) perchlorate reacts with acetone to give the RR-[Ni(L211)2] isomer, which is converted in pyridine exclusively into the / R-[Ni(L212)] + isomer [251]. Reaction of tris(propane-1,2-diamine) nickel(II) perchlorate prepared from racemic diamine with acetone affords C-rac and C-meso isomers of [Ni(L212)] + in approximately equal amounts [218, 251]. 

A soln. of thallic perchlorate prepared from thallic oxide and 60%-perchloric acid added to a soln. of p-cresol in methylene chloride, and vigorously stirred 5 min. at room temp. -> toluquinone. Y 70%. Also with y -acoxyethyl side chains s. Y. Yamada and K. Hosaka, Synthesis 1977, 53. 

The two ligands that have been most extensively studied are ortho-phenanth-roline and 2,2 -bipyridyl. Both of these ligands are bidentate and are only weakly basic. With ortho-phenanthroline the maximum number of bound ligands is four when the anion is the perchlorate ion (Krishnamurthy and Soundararajan, 1966). The tris-complex with one coordinated perchlorate ion (as indicated by the infrared spectrum) has also been obtained (Grandey and Moeller, 1970). There do not appear to have been any dipyridyl complexes with the lanthanide perchlorates prepared at the present time, although there does not seem to be any reason they would not form. 

As silica gel is known as a thermally stable material and can provide excellent thermal conductivity with the incorporation of salts, more studies were concentrated on silica compounds. Tatsumisago et aL reported on silica-gel films containing perchloric acid HCIO4, dodecatungstophosphoric acid and tetra-n-butylammonium perchlorate prepared by the sol-gel method using tetraethoxysilane. The films exhibited maximum conductivities of S/cm at room temperature (RT) with 19 wt% of HCIO4. 

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