【摘要】：本論文主要合成了四個(gè)SalenCo催化劑并比較了它們的催化活性,對(duì)在最佳的聚合條件下合成的聚合物進(jìn)行了表征及熱力學(xué)性能研究。本文還研究了合成的席夫堿及季銨鹽在常見(jiàn)的十幾種金屬離子中的識(shí)別效應(yīng)。具體的研究?jī)?nèi)容如下:通過(guò)以鄰甲酚為原料,經(jīng)過(guò)�；磻�(yīng)、加氫反應(yīng)、加醛反應(yīng)、換碘反應(yīng)和縮合反應(yīng)五個(gè)步驟合成了一種新型的Salen配體,并對(duì)合成條件進(jìn)行了優(yōu)化。通過(guò)正交實(shí)驗(yàn)探究了�；磻�(yīng)的最佳合成條件為反應(yīng)溫度-16℃,反應(yīng)物比例/n(鄰甲酚):n(三氯化鋁)=1/3.1,反應(yīng)時(shí)間為24小時(shí),產(chǎn)率為60.4%;加氫反應(yīng)的最優(yōu)條件為反應(yīng)溫度10℃,反應(yīng)物比例/n(化合物1):n(三乙基硅烷)=1/2.5,反應(yīng)時(shí)間為6小時(shí),產(chǎn)率為62%。在合成的Salen配體的基礎(chǔ)上與三乙胺反應(yīng)合成了含有四氟硼酸根的季銨鹽,通過(guò)改變季銨鹽上的陰離子合成了其他兩種季銨鹽分別含有醋酸根和硝酸根,用這三種季銨鹽與無(wú)水醋酸鈷絡(luò)合合成了一系列SalenCoX催化劑。研究發(fā)現(xiàn)含有2,4-二硝基酚的催化劑9(C9)催化活性最高,并優(yōu)化了最佳催化劑的聚合條件,其最佳的聚合條件為:聚合溫度為30℃、聚合壓力為2MPa、聚合時(shí)間為24小時(shí)。并且對(duì)最佳條件下四種催化劑催化合成的聚合物都進(jìn)行了表征及熱力學(xué)的研究,C9催化合成的聚合物為最佳,其玻璃化轉(zhuǎn)變溫度為-70℃,聚碳酸酯的含量也最高為0.583。同時(shí)采用凝膠滲透色譜(GPC)對(duì)本文中應(yīng)用合成的一系列催化劑催化合成的聚合物分子量的分布大小進(jìn)行了分析,并且通過(guò)核磁共振氫譜和紅外光譜表征了合成的各個(gè)化合物。本文還以合成的席夫堿和季銨鹽對(duì)常見(jiàn)的十幾種金屬離子(Na~+、K~+、Mg~(2+)、Al~(3+)、Zn~(2+)、Ag~+、Pb~(2+)、Co~(2+)、Li~+、Ba~(2+)、Ni~(2+)、Ca~(2+)、Cd~(2+)、La~(3+)、Cu~(2+)、Mn~(2+))進(jìn)行了離子識(shí)別的實(shí)驗(yàn)研究,通過(guò)紫外-可見(jiàn)吸收光譜對(duì)席夫堿和季銨鹽對(duì)金屬離子識(shí)別效應(yīng)進(jìn)行了實(shí)驗(yàn)測(cè)試,實(shí)驗(yàn)結(jié)果表明:席夫堿和季銨鹽兩者都對(duì)Zn~(2+)都有靈敏的識(shí)別性,而且選擇性較高。通過(guò)對(duì)紫外-可見(jiàn)吸收光譜進(jìn)行的濃度滴定,結(jié)果分析表明:席夫堿和季銨鹽與Zn~(2+)的絡(luò)合配比都是1:1。
[Abstract]:In this paper, four SalenCo catalysts were synthesized and their catalytic activities were compared. The polymer synthesized under the optimum polymerization conditions was characterized and its thermodynamic properties were studied. The recognition effects of synthetic Schiff bases and quaternary ammonium salts in more than a dozen metal ions were also studied. The main contents are as follows: a novel Salen ligand was synthesized by acylation, hydrogenation, aldehyde addition, iodization and condensation with o-cresol as raw material, and the synthesis conditions were optimized. The optimum conditions of acylation reaction were investigated by orthogonal experiment: reaction temperature-16 鈩，

本文編號(hào)：2394489