SU620484A1 - Method of obtaining peracids - Google Patents

Description

one

The invention refers to an improved method for producing percolation of the general formula

R-C-O-OH I

Oh where, -o-CgH

which are used for the floor; epoxy compounds.

A known method for producing percolate as well, in particular, perbenzoic acid, by reacting peroxide benzoyl with sodium alkoxide in toluene at. temperature minus 2 minus 5 ° C with stirring. To the resulting aqueous solution of sodium perbenzoate, concentrated hydrochloric acid is added. The free peracidum released by the action of H 5 O is extracted with chloroform 1.

The closest in technical essence to the proposed method is a method for producing peracids by reacting acyl peroxide

with an alcohol solution of an alkali metal hydroxide with the formation of a peracid salt and methyl e4ir cooraeiv. acid 21.

The resulting acid hydrolysis is converted into peracid.

The method is carried out as follows.

To a solution of potassium hydroxide in

Methyl alcohol, cooled to minus 7 ° C, is added with acyl peroxide and agitated until the peroxide is dissolved. Cool to minus and add cold water. The ester is extracted by CALCULUM chloroform. The hydroalcoholic layer is acidified with 2N sulfuric acid, and the peracid that separates out is extracted with chloroform. The yield of peracids is 59-83%.

After distilling off the solvent in vacuo, kristaplic oil is obtained, acid with a purity of no more than 90% 2.

Dp of obtaining a pure product requires additionally purification by sublimation in vacuum, for example dp synthesis

perbenzoic acid, or by recrystallization, in particular dp of o-cyclohexipmono-perioperative acid. These additional operations result in the loss of the product as a result of its decomposition and are explosive.

In addition, the perciptat yield for both these methods is relatively low.

The circuit of the invention is an increase in the output and purity of the perlspot.

This is achieved according to the proposed method for the preparation of percypot, a feature of which is the interaction of acyl peroxide with an alcohol solution of an alkali metal hydroxide in the presence of 0.1-2 mol. % Kokdaleksona-3 (ethylenediamine disodium salt of heteroacetic acid)

The resulting products are recovered by commonly known methods.

The ester is extracted with cold diethipic ether. The aqueous alcoholic solution is acidified with 2N sulfuric acid, and the peracid that separates out is extracted with chloroform. After distilling off the solvent in vacuo, crystalline percispot 99 is obtained, purity with yield 87–88; 5%

It has been established that small additions of Comppexone-3 significantly slow down the decomposition of the alkali salt of peracid, an intermediate product in the preparation of peracid by the proposed method.

The retarding effect of co-plexon-3 is due to the fact that traces of ions of variable valence metafields, which are always present as impurities in the reaction mixture, strongly catalyze the decomposition of the co-acid. The complexone captures metal ions in inactive 1compexes, eliminating the catalytic decomposition of the peracid salt. The addition of complexone-3 to the initial reaction mixture reduces the rate of decomposition of the peracid salt formed, thereby increasing the peracid output to 88% and the purity of D9 is 99.8%. No additional purification of the main product by sublimation or recrystallization is required.

In the examples given, the purity of the product obtained is characterized by. the content of active oxygen, defined iodometrically.

Example, a solution of 3.26 g (5.) KOH brand h and 0.2 g of complexon-3 in 10O mp of commercial methyl alcohol is cooled to minus and powdered 12.1 g stirring at a temperature of minus 7 C. The resulting solution is poured into a separating funnel containing 150 ml of distilled water and ice. form (4x50 ml); IXl the oroform extracts were combined, washed with cold distilled water (2 x 50 ml) and dried over calcined Na SCX. The solution was filtered, the solvent was removed from the filtrate in vacuum at room temperature. Bdg (88.5%) was obtained 99.8% oh perbenzoic acid.

Example2. o-Cyclohexyl monopergic acid is prepared analogously to example 1 from dicyclohexyl peroxydicarbonate, recrystallized from a mixture of methyl alcohols, od a (1: 1). Out of 14.3 g (5 1 1 O mol) peroxide, 6.95 g (87%) of 99.8% o-cyclohexyl mono-perugolic acid were obtained.

P (F implementation of the proposed method of obtaining peracids, provides the following benefits: B1:

the product yield (87-88.5%) compared with the yield (59-83%) according to a known method; an increase in the content of the main product to 99.8% compared to 90% according to a known method. In addition, no further purification of the peracid by sublimation or recrystallization is required, which simplifies the process of obtaining perispot, reduces product losses and eliminates explosive hazards.

Claims (2)

Invention Formula The method of obtaining peracid total formulas c-s-o-oi, where -, -0-С, by reacting an acidic peroxide with an alcohol solution of an alkali metal hydroxide at a temperature of minus 10 minus, followed by acid hydrolysis of an alkaline peroxide, and isolating the target products, characterized in that the interaction of an acidic peroxide 56204846 with an alcohol solution of hydroxide shchy-1, Weigand-Hipgetag. The methods of experimental metapp are carried out in the presence of organic chemistry: 0.1-2 MOS. % disodium sopi Egipen-M., 1968, p. 263. Dnamintetraacetic acid. 2. N. A. Sokopov, jap. A sliver Sources of information taken in 5 chemistry and chemical technology, attention in the examination: Bitter, no. 2, 1970, p. 45. Hydrocarbine acid peroxides. Corpses