Claims
- 1. A granular cross-linked polyarylene sulfide prepared 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 visocisty 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 granular cross-linked polyarylene sulfide of claim 1, wherein in step (B), said temperature raising rate is within the range of 20.degree. to 70.degree. C./hr.
- 3. The granular cross-linked polyarylene sulfide of claim 1, wherein, in step (B), said melt viscosity of the polymer obtained at 240.degree. C. is 700 to 5,000 poise.
- 4. The granular cross-linked polyarylene sulfide of 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 |
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Parent Case Info
This is a division of application Ser. No. 07/569,766, filed on Aug. 22, 1990, now U.S. Pat. No. 5,200,500. Which is a continuation of Ser. No. 07/352,879 filed May 17, 1989, now abandoned.
US Referenced Citations (17)
Foreign Referenced Citations (3)
Number |
Date |
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0166368 |
Jan 1986 |
EPX |
226998 |
Jul 1987 |
JPX |
256757 |
Feb 1988 |
JPX |
Divisions (1)
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Number |
Date |
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Parent |
569766 |
Aug 1990 |
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Continuations (1)
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Number |
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352879 |
May 1989 |
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