Studies on the Synthesis of Poly(phenylene sulfide) and Effect of Additives.

Abstract

Sodium sulfide(9H2O, SS)와 p-dichlorobenzene(DCB)을 단량체로 하고 N-methly-2-pyrrolidone(NMP)을 용매로 사용하여 poly(phenylene sulfide), PPS, 를 합성하였다. 이때 중합온도, 중합시간, 단량체의 stoichiometric rato 및 중합 첨가제들의 영향을 검토하였다. 중합수득율-시간 곡선 및 생성된 PPS 시료의 점도측정실험으로 부터 PPS중합반응은 reactive intermediate polycondensation의 특성을 나타냄이 관찰되었다. 중합반응의 적정온도는 250~270 ℃였으며 첨가제들의 종류에 따라 영향을 받았다. Lithium acetate는 중합속도 및 중합도를 증가시키나, lithium chloride는 감소시킴이 관찰되었다. Benzoquinone은 용매효과외에는 반응에 큰 영향이 없었다. 생성된 PPS시료는 IR 및 DSC 분석결과 표준시료들의 성질과 잘 일치하였다.

Poly(p-phenylene sulfides) were synthesized from sodium sulfide(9H2O) and p-dichlorobenzene in the N-methylpyrrolidone solvent. The effect of polymerization temperature, time, stoichiometric ratio of monomers and additives on the polymerization were studied. From the analysis of polymer conversion-time curve and viscosity of PPS samples, the polymerization reaction was found to deviate from the classical polycondensation. The polymerization reaction appeared to follow reactive intermediate polycondensation mechanism. The polymerization reaction was affected by the additives such as lithium acetate, lithium chloride and benzoquinone. While lithium acetate increased both polymeriation rate and degree of polymerization, lithium chloride decreased both of them. Benzoquinone added in the quantity ranging from 1/10 to 1 to the monomer concentration did not affect polymerization except changing the property of reaction solvent at high concentration.