铜酞菁的微波辐照法合成

The Synthesis of Copper Phthalocyanine under Microwave Irradiation

在微波辐照条件下 ,对铜酞菁的合成进行了研究。考察了辐照时间、尿素和氯化亚铜的用量、催化剂的种类及用量对铜酞菁产率的影响。发现在高功率微波辐照条件下 ,采用间歇辐照方式 ,以苯酐质量 3%的钼酸铵为催化剂 ,mol苯酐 ∶mol尿素 ∶mol氯化亚铜 =1∶ 5∶ 0 .2 0～ 0 .2 3,累计辐照 630 s,产率最高。若以氧化钼为催化剂 ,产率随其用量的增加而增加 ,并逐步趋向平稳 ,但催化效果不如钼酸铵。在相同原料配比条件下 ,微波法的产率比用常规的加热方法 ( 2 0 0℃ )高、反应时间短。两种方法所得产物的晶型经 X-射线粉末衍射分析均是β型为主 。

The synthesis of copper phthalocyanine under microwave irradiation was studied. The influence of the irradiation reaction time, the quantities of urea and copper chloride and the different catalysts on the yield of copper phthalocyanine were investigated. It was found that the yield reached the maxium under the intermittent microwave irradiation at high power for 630s with a certain reactant ratio(mol benzoic anhydrid ∶mol area ∶mol CH 2Cl =1∶5∶0.20~0.23) using ammonium molybdate as a catalyst (3wt% of benzoic anhydride). When the molybdenum oxide was selected as a catalyst, the yield increased with the increasing the quantity of the catalyst, then tended to be stationary. Under the selected same ratio of reactants, the yield of microwave method was higher than that of conventional heating means(200℃) with much shorter reaction time. X ray powder diffraction proved. The products of the two methods were mainly of β type, which was turned to α type after being refined by concentrated sulfuric acid.