SU220884A1 - METHOD OF OBTAINING POLYAMIDE - Google Patents

Description

This invention relates to the field of making polyamides in fine-grained form.

According to the invention, polyamides of aliphatic and cycloaliphatic dicarboxylic kielot in melkozerinstor form prepared by the condensation of diphenyl ether and k.islot aralifatichssknh or aliphatic diamines in equimolar amounts in an organic solvent without dissolving the polyamide at reflux temperature followed raetvoritel dokondensatsiey them by further heating at the same temperature or higher, but which is lower than the melting point of the polyamide, since otherwise particles forming polyamide will stick together. The degree of polymerization can be varied by varying the temperature and time of the heating heating, and the molecular weight indices are required to have a relative viscosity of 1.8 to obtain usable polyamide qualities.

After the end of the condensation, the fine-grained polyamide is separated from the suspension and washed easily with a volatile solvent, such as methanol, and sodate.

can be processed in pressure molding machines or bar presses. The invention is exemplified. Example 1. In a three-necked flask with a capacity of 750 mg, equipped with a stirrer, the reverse of the cold1: or 1k. With a funnel and thermometer, 24.2 g of diphenyloxalate (0.1 mol) are dissolved in 150 ml of diethylbenzene. With good stirring, they drip in for iriblizitelno IQ min in a nitrogen atmosphere and at a temperature of 180 ° C, 17.2 g of decamethleepiamine, dissolved in 50.yl diethylbenzene at 60 ° C. A fine precipitate falls out. It is stirred at the boiling point of the diagilbenzene still for 4 hours. After the reaction mixture has cooled, the polyamide powder is sucked off and washed repeatedly with a methapole. Polyamide powder is well dried. Relative viscosity 2.95. Temper; melting point of 275 ° C.

d p and m e p 2. Polyhexamethyldipipamide. In a three-necked flask, dissolve 29.8 g of phenyl adipate (0.1 mol) in 150 ml of benzene. Well stirring, vkanyvayut at a temperature of 80 ° C

A ratvor from 11.6 g of hexamethylenediamine (0.1 mol) in 50 ml of benzene. Once the mixture, from which, after a short time, the preliminary condensate in a fine-grained form falls, stir once more into a flowing flask, it is poured into an autoclave with a stirrer. Stirring, kondeisuyut further in a nitrogen atmosphere for 3 hours at a temperature of 170 ° C.

Further processing of the polyamide powder is the same as in Example 1. The relative viscosity is 2.06.

Example 3. Polyhexamethylenadinamide. 14.9 3 diphenylether of adinic acid (0.05 mol dissolved in 150 ml of dodecylbenzene. Stir well in nitrogen, drop the solution from 5.8 g of hexamethylenediamine in 50 ml of dodecylbenzene at 90 ° C for about 15 min. further within half an hour at a temperature of 90 ° C. Within 2-3 hours the temperature is raised to 190 ° C and at this temperature it is further condensed for another 3 hours.

Further processing of the polyamide powder is the same as in Example 1. The relative viscosity is 2.65.

Example 4. Polytetramethynesebacamide. 17.7 g of sebioic acid diphenyl ether (0.05 mol dissolved in 150 ml of diethylbeisol. Mix well under nitrogen and boil. For 15 minutes at 180 ° C, a solution of 4.4 g of tetramethylenediamine (0.05 mol in 50 ml of diethylbenzene At the same temperature, esh is condensed, and the polyagush powder is treated in the same manner as in Example 1 for 4 hours. The relative viscosity is 3.12.

Example 5. Polytetramethynesebacamide. As described in the irimer, 4, 38.2 g of sebacic acid cresol ester (0.1 mol) with 8.8 g of tetramethylenediamine (0.1 mol) are subjected to a decomposition reaction of 200 g of diethylbenzene. Relative viscosity is 2.26.

Example 6. Polytetramotileum and vacamid. As described in Example 4, 23.3 g of 6uc- (iper-6ytilphenyl) ester of sebacic acid (0.05 mol) with 4.4 g of tetramethylenediamine (0.05 mol) is subjected to an exchange decomposition reaction in 200 ml of diethylbenzene. The condensation temperature is maintained at 165 ° C. Otiositelia viscosity 1.89.

Example 7. Fullmethacrylenesebacemide. 17.7 g of sebacic acid diphenyl ether (0.05 mol) was dissolved in 150 ml of diethylbenzene. After stirring well at 80 ° C and under a nitrogen atmosphere, a solution of 6.8 g of L-xylylenediamine (0.05 mol) in 50 ml of diethylbenzene is instilled within 10 minutes. Then the temperature was raised to 160 ° C and then condensed further for 3 hours. The processing of the inoculated polyamide powder is the same as in Example 1. The relative viscosity is 1.82.

PRI me R 8. Fullhexameth. Chenhexahydroterephthalamide. 32.4 g of diphenylether of hexagndoterephthalic acid (0.1 mol) is dissolved in 150 ml of e 13ol. Stirring well at 80 ° C, add 10 g solution of 11.6 g of hexamethylenediamine to oQ ml of benzene for 10 n. In the course of 4 hours, they are stirred in boiling beisol, and then benzene is distilled off, and an equal volume of diethylbenzene is simultaneously dripped with irichem. The temperature in the reaction mixture thus slowly rises to 177 ° C. At this temperature, further iodine nitrogen is co-idled for an additional 5 hours. The subsequent treatment of the precipitated polyamide powder is the same as in Example 1. The gel viscosity is 2.18.

Subject invention

Method nolucheni polyamides grained form by polikoidepsatsii diphenyl ethers dikarboiovyh acids and aliphatic or araliphatic diamines in an organic solvent medium not dissolving the polyamide at the reflux temperature of the solvent followed dokoidensatsiey iutem heating at a temperature below the polyamide melting temperature, characterized in that as ester is used The dynethiyl esters of aliphatic or cycloaliphatic dicarboxylic acids.