Claims
- 1. A process to produce a cross-linked granular polyarylene sulfide by reacting an alkali metal sulfide, a dihaloaromatic compound and a polyhaloaromatic compound in an organic amide solvent, comprising:
- (A) an initial-stage polymerization step for obtaining a polyarylene sulfide by reacting an alkali metal sulfide, a mixture of dihaloaromatic and polyhaloaromatic compounds in an amount of 0.98 to 1.3 mol containing 0.003 to 0.1 mol polyhaloaromatic compound having three or more halogen substituents in a molecule, per mol of the alkali metal sulfide, in the presence of water in an amount of 0.5 to 2.9 moles per mol of said alkali metal sulfide at a temperature not lower than 180.degree. C. to lower than 235.degree. C. until a total conversion ratio of said dihalo- and polyhaloaromatic compounds reaches 50 to 98% and a melt viscosity of a polyarylene sulfide obtained at the end of the step becomes 5 to 5,000 poise, measured at 310.degree. C. and a shear rate of 1,200/second;
- (B) a temperature raising step in which with the amount of water adjusted to 2.5 to 7 moles per mole of fed alkali metal sulfide, the temperature raising condition from the temperature of step (A) to 240.degree. C. is controlled so that the melt viscosity of a polymer obtained at 240.degree. C. reaches in the range of 300 to 10,000 poise, measured at 310.degree. C. and a shear rate of 1,200/second and the temperature raising rate between 240.degree. C. and a temperature of the following step (C) is further controlled to be within the range of 10.degree. to 100.degree. C./hour; and
- (C) a second-stage polymerization step for further continuing the reaction at a temperature of 245.degree. to 290.degree. C. until a melt viscosity of the final product reaches not lower than 1.times.10.sup.5 poise, measured at 330.degree. C. and a shear rate of 2/second and wherein the average particle diameter of the granular cross-linked polyarylene sulfide obtained is 100 to 2,000 .mu.m.
- 2. The process according to claim 1, wherein in the step (B) said melt viscosity of a polymer obtained at 240.degree. C. is 700 to 5,000 poise.
- 3. The process according to claim 1, wherein in the step (B) said temperature raising rate is within the range of 20.degree. to 70.degree. C./hour.
- 4. The process according to claim 1, wherein in step (C), the amount of water at the second stage of polymerization is adjusted to within the range of 2.5 to 7 mols per mol of fed alkali metal sulfide.
Priority Claims (1)
Number |
Date |
Country |
Kind |
63-129390 |
May 1988 |
JPX |
|
Parent Case Info
This application is a continuation of application Ser. No. 07/352,879, filed on May 17, 1989, now abandoned.
US Referenced Citations (7)
Foreign Referenced Citations (3)
Number |
Date |
Country |
0166368 |
Jan 1986 |
EPX |
226998 |
Jul 1987 |
JPX |
256757 |
Feb 1988 |
JPX |
Continuations (1)
|
Number |
Date |
Country |
Parent |
352879 |
May 1989 |
|