Process for the preparation of cross-linked polyarylene sulfide

Details Process for the preparation of cross-linked polyarylene sulfide Process for the preparation of cross-linked polyarylene sulfide

C - Chemistry, Metallurgy

08

G

402/344

C08G 75/02 (2006.01)

Patent

CA 1337837

The present invention discloses a process for producing a granular polyarylene sulfide which has a high melt viscosity and a high degree of cross-linkage, becomes gel under melting and is easy to handle in the production and the fabrication thereof. The process disclosed herein comprises (1) a step (A) an initial-stage polymerization step for obtaining a polyarylene sulfide by reacting an alkali metal sulfide, a dihaloaromatic compound and a polyhaloaromatic compound, having three or more halogen substituents in a molecule, in the presence of water in an amount of 0.5 to 2.9 moles per mole of said alkali metal sulfide at a temperature in the range of 180 to 235°C until the total conversion ratio of said dihalo- and polyhaloaromatic compounds reaches 50 to 98% and the melt viscosity of a polyarylene sulfide obtained at the end of the step becomes 5 to 5,000 poise, measured at 310°C and a shear rate of 1,200/second; (2) a step (B) a temperature raising step in which while adjusting an amount of water to be 2.5 to 7 moles per mole of fed alkali metal sulfide, a temperature raising condition from the temperature of step (A) to 240°C is controlled so that the melt viscosity of a polymer obtained at 240°C reaches 300 to 10,000 poise, measured at 310°C and a shear rate of 1,200/second and the temperature raising rate between 240°C and a temperature of the following step (C) is further controlled to be within the range of 10 to 100°C/hour; and (3) a step (C) a second-stage polymerization step for further continuing the reaction at a temperature of 245 to 290°C until a melt viscosity of the final product reaches not lower than 1 x 105 poise, measured at 330°C and a shear rate of 2/second. The present invention also discloses a granular cross-linked polyarylene sulfide produced by the process described above.

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