SU1261937A1 - Method of producing n,n'-bis-(furfuryliden)-1,6-diaminohexane - Google Patents

Abstract

THE METHOD OF OBTAINING N, N -BHC (FURFURILIDENE) -, 6-DIAMINOHEXANE by the interaction of furfurol with hexa-methylenediamine in aqueous solution at 0-5 C, followed by washing and drying, characterized in that, in order to increase the shelf life of s, bis- (furfurylidene) 1, 6-diaminohexane, the process is carried out in the presence of 2,2,6,6-tetra-methyl-4-oxopiperP din-N-oxide, taken in an amount of 0.1-0.15% by weight of the target product.

Description

The invention relates to an improved process for the preparation of N, N-6Hct (furfurylidene) -, 6-diamino hexane (bifurgin), which is used as a vulcanizing agent. The aim of the invention is to increase the shelf life of bifurgin. Example 1. A chemical composition with a capacity of 0.5 l is placed in a bath filled with a mixture of ice and sodium chloride, which provides a temperature of up to. The glass is equipped with an electric stirrer and a mercury thermometer with a temperature measuring range from -10 to +30 C. The glass is placed 24 g freshly distilled, the stirrer is turned on and 214 ml of a 20% aqueous solution of hexamethylenediamine are poured in small portions so that the temperature in the glass does not exceed 0-5 C. After 15 minutes, when the dosage of the hexamethylenediamine is completed, the stirrer is turned off. The resulting product is subjected to repeated washing with water, followed by filtration and drying. EXAMPLE 2. A 0.5 liter beaker is placed in a bath filled with a mixture of ice and sodium chloride, which provides a temperature to the supply cup; an electric stirrer with a mercury thermometer with a temperature measurement range of -10 to + 30s . 24 g of freshly distilled furfural are placed in a glass, the stirrer is switched on and 2.4 mg of the inhibitor 2,2,6,6-tetrame tyl-4-oxopiperidine N-oxide is dosed out, keeping the contents to the temperature (± 2 ° C) 2I4 ml of a 20% aqueous solution of hexamethylenediamine is poured into small glasses in such a way that the temperature in the glass does not exceed 0-5 C. After 15 min after the completion of the dosage of the aqueous solution of hexamethylenediamine, the agitator is turned off. The resulting product is subjected to multiple washing followed by filtering and drying. Example 3. Chemical A 0.5 L glass beaker is placed in a bath filled with a mixture of ice and sodium chloride at a temperature of up to -10 ° C. The glass is equipped with an electric stirrer with a mercury thermometer 7 with a temperature measuring range of -10 to +30 C. The glass is placed 24 g of freshly distilled furfural, turn on the stirrer and dispense 24 mg of the inhibitor — 2,2,6,6-tetrameish-1 to 4 oxopiperidine-K-oxide, keeping the contents until the temperature reaches - (8 ±. 2) ° C. After that, 214 ml of a 20% aqueous solution of hexamethylenediamine is poured into small glasses in such a way that the temperature in the glass does not exceed 0-5 ° C. After 15 minutes, upon completion of the dosage of an aqueous solution of hexamethylenediamine, the stirrer is turned off. The resulting product is subjected to repeated washing with water, followed by filtration and drying. EXAMPLE 4 A 0.5 l beaker is placed in a bath filled with a mixture of ice and sodium chloride at a temperature of -10 ° C. The glass is equipped with an electric stirrer with a mercury thermometer with a temperature measurement range of -10 to +30 ° s 24 g of freshly distilled furfural are placed in a beaker, the stirrer is switched on and 36 mg of the inhibitor 2,2,6,6-tetramethyl-4-oxopiperidine-M-oxide is dispensed, released, and the content is kept until the temperature reaches (8 + 2 ° C) 214 MPs of 20% aqueous hexamethylenediamine solution are poured into small glasses in such a way that the temperatures in the glass do not exceed 0-5 C. After 15 min after the completion of the dosage of the aqueous solution of hexamethylenediamine, the agitator is turned off. subsequent filtering and noun Example 5. A 0.5 L chemical beaker is placed in a bath filled with a mixture of ice and sodium chloride at a temperature of -10 ° C. The glass is equipped with an electric stirrer with a mercury thermometer with a temperature measurement range of -10 to + 30s 24 g of freshly distilled furfural are placed in a beaker, the stirrer is switched on and 43 mg of the inhibitor 2,2,6,6-tetramethyl-4-oxopypervdin-K-oxide is metered into the beaker, holding the content until the temperature reaches (8 + 2) ° С . After that, 214 ml of a 20% aqueous solution of hexamethylenediamine is poured into small glasses in such a way that the temperature in the glass does not exceed 0-5 ° C. After 15 minutes, upon completion of the dosage of an aqueous solution of hexamethylenediamine, the stirrer is turned off. The resulting product is subjected to repeated washing with water followed by filtration and drying. Sample K, M-bis- (furfurylidene) I, 6-diaminohexane, stabilized during the synthesis of 2,2,6,6-tetramethyl-4-oxopiperidine-M -oxide, kept in an airtight container at 40 ± 2 ° C for 68 days, which corresponds to 9 months of storage at 20 s. The results of the experiments are presented in the table. 374 After 68 days of testing at 40 C N, N-bis- (furfurylidene) -1,6-diamino-. hexane with a stabilizer retains a yellow-brown color, and so on. not less than 44.3 C in accordance with the specifications. T The technical and economic efficiency of the invention is determined by a significant reduction from 3 to 9 months - the duration of preservation of the quality indicators N, N of bis- (furfurylidene) -1, b-diaminohexane stabilized by 2,2,6,6-tetrametnp 4-oxopiperidine-N-oxide. An increase in the storage period of N.N. bis- (furfurylidene | -1,6-diaminohexane) eliminates its losses during storage and contributes to an increase in the quality and storage time of rubber based on fluororubber.

ABOUT

0.01

0.10

0.15

0.18

g45,5

Does not match

brown 45.4 44.4

brown

Complies with 44.3

 II 44.3

Claims (1)

METHOD FOR PRODUCING Ν, Ν -BIS (FURFURYLIDENE) -1,6-DIAMINOHEXANE by reacting furfural with hexa · methylenediamine in an aqueous solution at 0-5 ° C followed by washing and drying, characterized in that, in order to increase the shelf life of I ^ ' -bis- ^ urfuriliden) - 1,6-diaminohexane, the process is carried out in the presence of 2,2,6,6-tetraethyl-4-oxopiperidin-I-oxide, taken in an amount of 0.1-0.15% by weight of the target product.