SU414268A1 - - Google Patents

Description

one

This invention relates to a method for the preparation of organophosphorus compounds, namely the mixture of MONO- and dialkyl phosphate esters, which are used as extractants, antioxidants, surface-active substances, etc.

A method is known for producing a mixture of mono- and dialkyl esters of phosphoric acid by reacting phosphoric acid with snartami in the presence of boric acid and sintering as a catalyst.

The disadvantage of this method is the use of boric acid, which complicates the process technology.

With the elimination of this drawback, it is proposed to withdraw the acid-type ion-exchange resin as a catalyst, which is an industrial catalyst that is easily regenerated and can be successfully used.

With siTOM, the equipment is practically corroded and the process can be carried out continuously.

The reaction is usually carried out with heating, preferably up to the temperature of the hip and the mixture of starting materials, followed by isolation of the target product using methods.

Example 1. Esterification of phosphoric acid with octyl alcohol.

A mixture of 71.5 g (0.55 g-mol) of octyl alcohol, 57.6 g (0.5 g-mol) of 85% -iioi i phosphoric acid, 10 g of cation exchanger KU-2 in the I-form and 500 ml of toluene boil in a Dean-Stark device until water stops (13 hours), cool, filter KU-2, from the filtrate after removing the solvent. 104.8 g of crude product are obtained; its content according to potentiometric titration is 56.2% monoalkyl phosphate and 31.8% dialkyl phosphate. The yield of the mixture of mono- and dioctyl phosphates, based on the starting alcohol, is 89.6%. The phosphate mixture is treated with aniline, recrystallized from ethyl alumina, and the aniline salt of monooctyl phosphate is obtained, m.p. 129-131 ° C. (according to literature data, pl. 129-130 ° С).

Found,%: C 55.7; H 8.9; N 4.8; R 10.5.

NO4P Sib.

Calculated,%: C 55.4; H 8.62; N 4,6; R 10.2.

Example 2. Esterification of phosphoric acid with dodecyl alcohol.

A mixture of 39 g (0.5 mol) of a pre-dopil acid solution, 69.0 g (0.6 mol) of 85% phosphoric acid, 10 g of Kin-2 KU-2 and 500 ml of toluene at a Dean-Stark device until the release of water (15 hours), cooled, KU-2 is filtered off and from the filtrate, after removal of the solvent, 124 g of product are obtained, containing, according to potentiometer 3 of the titrea, 89.5% of my ophthalate and | () Dopedyl ( ос; osfate. The yield of M0110-II didodoscyl phosphate based on the initial alcohol is 94.1%. -., Subject and rectification 1. The method of obtaining a mixture of phospholipopropyl methyl esters isosta by the interaction of phosphoric acid eo with alcohols at 4 Glpfg-; piii to the presence of a catalyst followed by extraction of the Pslg product from the ingest methods; iii, and ii c and the fact that 2. The method according to claim 1, dated by the fact that the process is carried out at temcerature. There is an injection of a mixture of starting reagents.