Process for preparing poly(sulfonyl-phenylene)phenylphosphonate
First Claim
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1. A PROCESS FOR PREPARING POLY(SULFONYLDIPHENYLENE)PHENYLPHOSPHONATE WHICH COMPRISES POLYCONDENSING DIHYDROXYDIPHENYLSULFONE AND PHENYLPHOSPHONICC DICHLORIDE IN TETRACHLOROETHANE, DECREASING THEVISCOSITY OF THE RESULTING SOLUTION BY ADDNG 0.1 -2.5% OF METHANOL BASED ON TOTAL SOLVENT AND ADDING THE SOLUTION TO A METHANOL BATH TO PRECIPITATE POLY(SULFONYLDIPHENYLENE)PHENYLPHOSPHONATE.
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Abstract
Poly(sulfonyldiphenylene)phenylphosphonate is prepared in solution by polycondensing dihydroxy-diphenylsulfone and phenylphosphonic dichloride in tetrachloroethane. The viscosity of the resulting solution is decreased by adding 0.1 to 25% of methanol and the polymer may be precipitated from solution by adding said solution to a methanol bath.
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8 Claims
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1. A PROCESS FOR PREPARING POLY(SULFONYLDIPHENYLENE)PHENYLPHOSPHONATE WHICH COMPRISES POLYCONDENSING DIHYDROXYDIPHENYLSULFONE AND PHENYLPHOSPHONICC DICHLORIDE IN TETRACHLOROETHANE, DECREASING THEVISCOSITY OF THE RESULTING SOLUTION BY ADDNG 0.1 -2.5% OF METHANOL BASED ON TOTAL SOLVENT AND ADDING THE SOLUTION TO A METHANOL BATH TO PRECIPITATE POLY(SULFONYLDIPHENYLENE)PHENYLPHOSPHONATE.
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2. The process of claim 1, wherein the water content of the dihydroxydiphenylsulfone is decreased to less than 1 mole % by azeotropic distillation of the mixture of dihydroxydiphenylsulfone and tetrachloroethane, before the polycondensation.
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3. The process of claim 1, wherein the solution of poly(sulfonyldiphenylene)phenylphosphonate in tetrachloroethane is added gradually to methanol under conditions of the stabe dispersing zone shown in FIG. 1.
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4. The process of claim 1, wherein said polycondensation is effected in contact with a catalyst of magnesium chloride or calcium chloride.
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5. The process of claim 1, wherein the molar ratio of phenylphosphonic dichloride to dihydroxydiphenylsulfone in the polycondensation is 0.9 to 1.1, preferably 0.99 to 1.01.
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6. The process of claim 1, wherein the weight ratio of tetrachloroethane to the resulting poly(sulfonyldiphenylene)phenylphosphonate in the polycondensation is more than 2.
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7. The process of claim 1, wherein the said polycondensation is carried out at the reflux temperature of tetrachloroethane.
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8. The process of claim 1, wherein the degree of polymerization of the poly(sulfonyldiphenylene)phenylphosphonate is more than 6.
Specification