摘要
以乙醇为溶剂，3，5-二叔丁基水杨醛与2，6-二异丙基苯胺通过希夫碱缩合得到3，5-二叔丁基水杨醛缩2，6-二异丙基苯胺配体Ia，收率92．5％。配体Ia在四氢呋喃中分别与NaH和TiCl4·2THF反应得到相应的水杨醛亚胺钛配合物I。气相色谱-质谱联用（GC／MS）表征了配体结构，核磁共振氢谱（^1HNMR）、元素分析等手段表征了配合物I。以甲苯为溶剂、MAO（甲基铝氧烷）为助催化刑，在25～75℃钛配合物I催化乙烯聚合活性较高（1．080×10^5～1．986×10^6g PE·（mol Ti）^-1·h^-1），在55℃达到最高。所得聚乙烯粘均分子量在13．1×10^4～60．5×10^4之间，反应压力从0．2MPa提高到1．0MPa，I／MAO催化体系活性和聚合产物分子量能大幅提高。GPC和DSC表征结果说明所得聚合物为窄分布低支化度聚乙烯。
Reaction of 3,5-di-t-butyl-salieylaldehyde with 2,6-di-isopropyle-aniline via Schiff base condensation in ethanol afforded the corresponding phenoxy-imine ligand Ia with 92.5% yield. Ligand Ia was characterized by mass Spectra. Treatment of this ligand with Nail and TiCl4·2THF in THF respectively, a new complex bis[-N-（3,5-di-tert-butylsalicylidene）-2,6- diisopropylanilinato] titanium （IV） dichloride （I） was obtained and its structure was characterized by ^1HNMR and elemental analyses. Aetivated by MAO, Complex I displayed very high activity for ethylene polymerization. Under the conditions of 25～75℃ and 0.2～1.0 MPa, the activities achieved （1.080×10^5～1.986×10^6）g PE·（mol Ti）^-1·h^-1 and the viseometric average molecular weight （Mv） of polyethylene was between 13.1×10^4～60.5×10^4. The activities and the My increased with the pressure from 0.2 MPa to 1.0 MPa. The temperature＇s effect on activity of complex I was very strong. The data characterized by GPC and DSC showed the synthesis of linear polyethylene （LPE）.
出处
《化学与生物工程》
CAS
2006年第3期10-12,共3页
Chemistry & Bioengineering
基金
湖北省教育厅技术创新项目(J200511001)
关键词
水杨醛亚胺
钛配合物
乙烯聚合
催化剂
salicylaldimine
titanium complex
ethylene polymerization
catalyst
