A METHOD FOR THE PREPARATION OF POLY(PHENYLENE SULFIDE)
A method for the preparation of poly(phenylene sulfide) involves a reaction between an alkaline metal hydrosulfide and 1,4-dichlorobenzene in a polar solvent. It is carried out such that the alkaline metal hydrosulfide and hydroxide are dissolved in water and mixed, and then N-methylpyrrolidone and...
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Format | Patent |
Language | English French |
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07.10.2021
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Abstract | A method for the preparation of poly(phenylene sulfide) involves a reaction between an alkaline metal hydrosulfide and 1,4-dichlorobenzene in a polar solvent. It is carried out such that the alkaline metal hydrosulfide and hydroxide are dissolved in water and mixed, and then N-methylpyrrolidone and additives that ensure an adequate reaction medium are added, and excess water is removed by distillation. A silicate suspension in a solution of 1,4-dichlorobenzene with N-methylpyrrolidone is added to the thus obtained system, wherein the mean silicate grain size is not higher than 10 µm. Then, polycondensation is carried out for 2 to 10 hours at a temperature ranging from 220 to 270 ºC, and a post-reaction mixture is obtained, from which a polymer is separated, which is in turn purified and dried. A material with high molecular weight and a high degree of crystallinity is obtained with a good yield.
Procédé de préparation de poly(sulfure de phénylène) impliquant une réaction entre un sulfhydrate de métal alcalin et du 1,4-dichlorobenzène dans un solvant polaire. Le procédé est mis en œuvre de telle manière que le sulfhydrate de métal alcalin et l'hydroxyde sont dissous dans de l'eau et mélangés, puis sont ajoutés de la N-méthylpyrrolidone et des additifs qui garantissent un milieu réactionnel approprié, l'excédent d'eau étant éliminée par distillation. Une suspension de silicate dans une solution de 1,4-dichlorobenzène avec de la N-méthylpyrrolidone est ajoutée au système ainsi obtenu, la granulométrie moyenne du silicate n'étant pas supérieure à 10 µm. Une polycondensation est ensuite mise en œuvre pendant 2 à 10 heures à une température dans la plage de 220 à 270 °C, ce qui produit un mélange post-réactionnel, dont un polymère est séparé, lequel est ensuite purifié et séché. Le procédé génère un bon rendement d'un matériau ayant une masse moléculaire élevée et un degré élevé de cristallinité. |
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AbstractList | A method for the preparation of poly(phenylene sulfide) involves a reaction between an alkaline metal hydrosulfide and 1,4-dichlorobenzene in a polar solvent. It is carried out such that the alkaline metal hydrosulfide and hydroxide are dissolved in water and mixed, and then N-methylpyrrolidone and additives that ensure an adequate reaction medium are added, and excess water is removed by distillation. A silicate suspension in a solution of 1,4-dichlorobenzene with N-methylpyrrolidone is added to the thus obtained system, wherein the mean silicate grain size is not higher than 10 µm. Then, polycondensation is carried out for 2 to 10 hours at a temperature ranging from 220 to 270 ºC, and a post-reaction mixture is obtained, from which a polymer is separated, which is in turn purified and dried. A material with high molecular weight and a high degree of crystallinity is obtained with a good yield.
Procédé de préparation de poly(sulfure de phénylène) impliquant une réaction entre un sulfhydrate de métal alcalin et du 1,4-dichlorobenzène dans un solvant polaire. Le procédé est mis en œuvre de telle manière que le sulfhydrate de métal alcalin et l'hydroxyde sont dissous dans de l'eau et mélangés, puis sont ajoutés de la N-méthylpyrrolidone et des additifs qui garantissent un milieu réactionnel approprié, l'excédent d'eau étant éliminée par distillation. Une suspension de silicate dans une solution de 1,4-dichlorobenzène avec de la N-méthylpyrrolidone est ajoutée au système ainsi obtenu, la granulométrie moyenne du silicate n'étant pas supérieure à 10 µm. Une polycondensation est ensuite mise en œuvre pendant 2 à 10 heures à une température dans la plage de 220 à 270 °C, ce qui produit un mélange post-réactionnel, dont un polymère est séparé, lequel est ensuite purifié et séché. Le procédé génère un bon rendement d'un matériau ayant une masse moléculaire élevée et un degré élevé de cristallinité. |
Author | KOCZWARA, Zbigniew ELIAS, Bernard SNOPKIEWICZ, Zbigniew ROBASZKIEWICZ, Andrzej WARZAŁA, Marek SEMENIUK, Izabela MISKA, Marcin STAŃCZYK, Dorota NOWICKI, Janusz KRZYSIAK-WARZAŁA, Barbara CZERW, Rafał PIEŃKOWSKI, Kamil STEMPIŃSKI, Edward MIJAŁ, Witold MAZUR, Marta MOŁAS, Elżbieta NOSAL, Hanna NOWAKOWSKA-BOGDAN, Ewa MATUS, Grzegorz LEDNIOWSKA, Kerstin KANIA, Jan KUDŁA, Stanisław |
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Title | A METHOD FOR THE PREPARATION OF POLY(PHENYLENE SULFIDE) |
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