SU471356A1 - Purification method of 2,2 "-dioxy-3,3", 5, 5 ", 6,6" -hexachlorodiphenylmethane - Google Patents

Description

I

The invention relates to a purification method for 2,2-dioxy-3,3,5,5,6,6-hexachlorodiphenylmethane (hexachlorophene), used as a bactericidal and antihelminthic irenarate.

A known method of purification of hexachlorophene, obtained by exposure to 2,4,5-trichlorfsnola with formaldehyde in an acidic medium and containing as impurities trphlorobenzdioxolane-1, 3 and other by-products of sietez. In this purification process, the technical hexachlorophores are dissolved at 100 ° C in an aqueous solution of caustic water, activated carbon is added, filtered, the filtrate is acidified to a pH of 10.3 at, cooled down, and the hexachlorophosphoride salt is filtered.

Hexachlorophene monosodium salt is sprinkled with cold water and suspended in an eight-cratio amount of distilled water, heated to 50 ° C, and ochi1, enny 1 hexachlorophene with m.il. 165-166 ° C. The yield of the target product 58-60% of theoretical.

The aim of the invention is to increase the yield and quality of the target product.

To do this, the ionic salt of 2,2-dioxy3, 3,5,56,6-hexachlorodifeiylmetaia is treated with an aqueous solution of caustic acid and sodium to a pH of 12-13, followed by treatment with loluchein while disodium salt 2,2 dioxy - 3, 5.6.6 - hexachlorodifeiylmethane with activated carbon in the presence of sodium bisulfite and zinc dust (active 5tel reducing) and release of the desired product by known methods.

The yield of the target product 94.5% of theoretical. Purified hexa. Chlorophene has m. Pl. 166.5-166 ,.

PR and L1 e r. 25 g of technical hexachlorophene are dissolved at 100 ° C in 100 ml of a 12.3% solution of caustic acid and the solution is filtered. The filtrate is adjusted to pH 10.5 at 50 ° C with sulfuric acid. The monoacrylate salt of hexachlorophene is formed and filtered and dissolved in 100 ml of i2.3% -rioro caustic solution of sodium hydroxide (pH 12-13), 1 g of activated carbon, 1.5 g of bisulfite, rp is added (and 100 g %) and 0.3 g of zinc dust, unmixed for 0.5-1 hours, and the solution is fired at. The filtrate is cooled to 50 ° C and bottoms are reduced to pH 10.5. The purified sodium salt is filtered off, tromped with water and suspended in a bristle amount of water, the acid is added to a blue koigo stain. filter, cozy sediment, washed with water until neutral but Congo dried. Vygehsachlorofena

with t. il. from teoreg or 34

The subject matter of the invention is the yield and quality of the target product, its method of purification of 2,2-d110xy-3,35,5,6,6-hexane sodium hydroxide to pH 12-13 with

Saclorodiphenylmethane from trichlorobenzdioxo and subsequent treatment with this method

lana-1,3 by treatment with an aqueous solution5 of the disodium salt of 2,2-dioxy-3,3,5,5,6,6-hexed sodium at the increased temperature of ssachlorodiphenylmethane with activated carbon

the preparation of 2,2-dioxy-monosodium salt in the presence of sodium bisulfite and zinc

3,3,5,5,6,6-hexachlorodiphenylmethane, about a liter of dust and extraction of the target product with lime u {and so that, with the aim of increasing by means of methods.

471356

sodium salt is treated with water