Abstract:
The invention comprises triarylmethane dyes having the formula in which R1 denotes a low molecular weight alkyl group, R2 and R3 are hydrogen atoms or aliphatic, cycloaliphatic, aliphatic-cycloaliphatic radicals which may be connected to form a fused cycloaliphatic ring, and Y is a chlorine or bromine ion. The dyes of the above formula are made by condensing together p,p1-bisdialkyl-aminobenzophenones of formula with a secondary amine having the formula in the presence of a condensing agent containing chlorine or bromine. In formulae III and IV, R1, R2 and R3 have the meanings as above; as condensing agents phosphorus trichloride, tribromide, pentachloride, oxychloride, oxybromide and phosgene are specified. The reactions are carried out in inert solvents, e.g. toluene and xylene, and the dyes produced have good solubility in alcohol and castor oil.
Abstract:
Chlorinated isocyanuric acid is produced by leading Cl2 into an aqueous solution of sodium or potassium cyanurate until the pH is less than 7, adding an alkali compound, i.e. sodium or potassium hydroxide, carbonate, or bicarbonate, preferably in aqueous solution, in amount equivalent at most to 30% of the free and combined cyanuric acid, and continuing addition of Cl2 until the pH is 5 to 2.5.5-20% solutions of di- Na or K cyanurate or tri- Na or K cyanurate produce pure di- or tri-chloroisocyanuric acid respectively. A mixture of di- and tri-chloroisocyanuric acids may also be prepared. The reaction may be effected at normal or elevated pressure at temperatures below 100 DEG C., preferably below 50 DEG C. for di-chloro-acid and below 40 DEG C. for tri-chloro-acid, particularly -10 DEG to 35 DEG C. The reaction may be in the presence of water-miscible liquids, e.g. methanol, ethanol, acetone, acrylonitrile, aliphatic or aromatic amines, phenols, urea, or formaldehyde. Addition of the alkali compound may be all at once, periodically, or continuously, and the further addition of Cl2 may be during and/or after the alkali compound. The solid crystalline chlorinated isocyanuric acid may be separated from the reaction mixture mechanically, and washed with water, and the mother liquor and washings may be reused in the process. The acid may be dried below 100 DEG C. preferably at below 50 mm. Hg. pressure. Alternatively, the acid may be dried by treating with water-immiscible organic liquids, e.g. benzene or carbon tetrachloride, preferably at below 50 DEG C. in vacuo. Decomposition of the acids or their salts may be inhibited by adding formaldehyde, or salts of phosphorus acid or of hydroxylamines.
Abstract:
Cyanuric acid is obtained by eliminating ammonia from urea in hot diphenyl, diphenyl oxide, or a halogen substitution product thereof having up to two halogen atoms in each phenyl nucleus, i.e. from one to four halogen atoms in the molecule. Temperature may be 220-300 DEG C., and pressure reduced, elevated or atmospheric. A reaction temperature is preferably chosen at about the boiling point of the hot liquid at the pressure employed. Mixtures of diphenyl compounds may be used which have a melting point from 10-30 DEG C. Other liquids referred to are bromodiphenyls, chloro-diphenyls, and dichlorodiphenyl.
Abstract:
Pure chlorendic acid [1,4,5,6,7,7-hexachlorobicyclo-[2,2,1]-heptene - (5) - dicarboxylic acid-(2,3)] is prepared by reacting hexachlorocyclo pentadiene and maleic anhydride in a solvent at 120-200 DEG C., hydrolysing the chlorendic acid anhydride, and treating the resulting chlorendic acid with an aqueous solution of an aliphatic carboxylic acid containing up to 6 carbon atoms, preferably at a temperature between room temperature and 40 DEG C. Specified acids are formic, acetic, propionic, butyric, isobutyric, valeric, isovaleric and acrylic acids, and acids containing inert substituents, e.g. halogen atoms or alkoxy groups, such as chloracetic acid, dichloracetic acid, and lactic acid methyl ether. The preferred acid concentration is 2-15% by weight, and generally the acid solution is used in amounts of half to twice the weight of chlorendic acid. The treatment may be in a heterogeneous system, by moistening or suspending the chlorendic acid with or in the aqueous acid solution and filtering, or in a homogeneous system, the amount of aqueous acid and its temperature being such that the chlorendic acid passes completely into solution and crystallises out on cooling. The purification step may be combined with the hydrolysis step by carrying out the hydrolysis with the aqueous carboxylic acid solution. Specifications 614,931 and 855,586 are referred to.