減壓輔助法制備PPDO
本文選題:聚對二氧環(huán)己酮 切入點:辛酸亞錫 出處:《材料科學(xué)與工程學(xué)報》2016年01期 論文類型:期刊論文
【摘要】:本文以辛酸亞錫(Sn(OCt)_2)為催化劑,乙二醇為引發(fā)劑,首次采用減壓輔助法合成聚對二氧環(huán)己酮(Poly(p-dioxanone),PPDO),并系統(tǒng)研究了引發(fā)劑、減壓時間及引發(fā)時間對聚合反應(yīng)的影響。利用紅外光譜(IR)、核磁光譜(~1H NMR)、特性粘度(η)、X射線廣角衍射(WAXD)及差示掃描量熱法(DSC)對聚合產(chǎn)物的結(jié)構(gòu)及熱力學(xué)性能進(jìn)行初步探討。IR、~1H NMR及WAXD測試結(jié)果表明:減壓法能夠得到高純度且晶型相同的PPDO產(chǎn)物。且在減壓12h時,單體轉(zhuǎn)化率達(dá)到最大值(86.5%)。引發(fā)6h時,單體轉(zhuǎn)化率達(dá)到84.5%。而未加引發(fā)劑時,單體轉(zhuǎn)化率僅為81.1%。DSC測試結(jié)果表明:產(chǎn)物的熔融溫度(T_m)與結(jié)晶溫度(T_c)均隨減壓時間及引發(fā)時間的延長呈現(xiàn)先上升后降低的趨勢。相比傳統(tǒng)方法,減壓輔助法能夠獲得更高的產(chǎn)率。同時有效地避免了溶解-沉淀提純而引入的雜質(zhì)。
[Abstract]:In this paper, Poly (p-Dioxanone) PPDOO _ (2) was synthesized by decompression assisted method with Sn-Sn-OCtO _ (2) octanoate as catalyst and ethylene glycol as initiator, and the initiator was studied systematically. The effect of decompression time and initiation time on the polymerization reaction. The structure and thermodynamic properties of the polymerization products were studied by IR, 1H NMR, WAXD and DSCS. The results of 1H NMR and WAXD test showed that the PPDO products with high purity and the same crystal form could be obtained by decompression method, and at 12 h of decompression, The monomer conversion reached the maximum value of 86.5% and reached 84.5% when the monomer was initiated for 6 h. When the initiator was not added, the monomer conversion reached 84.5%. The results of DSC test showed that both the melting temperature and crystallization temperature of the product increased first and then decreased with the prolongation of the decompression time and initiation time, compared with the traditional method, the monomer conversion was only 81.1% and the DSC test showed that the melt temperature and crystallization temperature of the product increased first and then decreased with the prolongation of the decompression time and initiation time. The vacuum assisted method can obtain higher yield and effectively avoid the impurities introduced by solution-precipitation purification.
【作者單位】: 四川大學(xué)物理科學(xué)與技術(shù)學(xué)院;
【基金】:國家國際科技合作專項資助項目(2013DFB50280)
【分類號】:TQ317
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