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合成铜酞菁染料
摘要 本论文研究了以苯酐、尿素、氯化亚铜、钼酸铵为原料,微波辐照法和传统固相法合成铜酞菁染料这一课题。通过改变反应温度、反应时间、及原料配比得出合成铜酞菁的最佳方案,并从各个角度对两种方法进行了比较,最后对两种方法合成的铜酞菁产品进行检测分析,比较两种产品的质量。微波辐照法中,主要考察了辐照时间、尿素用量、氯化亚铜用量、苯酐用量、钼酸铵用量对铜酞菁产率的影响,得出此法合成铜酞菁的最佳配比为苯酐:尿素:氯化亚铜(摩尔比)=1:5:0.21,钼酸铵的用量为苯酐重量的4%。传统的方法合成铜酞菁时,应将反应温度控制在210~220℃之间,反应时间应控制在2小时左右为宜。通过比较两种方法得出,微波辐照法反应速率快,反应时间短,产率高,产品质量好,污染少,比传统方法优越。两种方法得到的产品性质基本相同,其晶型均以β型为主,经浓硫酸精致以后转变为为α型。 关键词:铜酞菁;微波辐照;传统固相法;苯酐;尿素;氯化亚铜;钼酸铵;催化 Abstract The synthesis of copper phthalocyanine under microwave irradiation and conventional heating means In this paper,the synthesis of copper phthalocyanine by the reaction of benzonic anhydride,urea,ammonium molybolenum and catalyst under microwave irradiation and classical method were studied mostly.It was found the best synthesis conditon of copper phthalocyanine through changing reaction time,reaction temperature ,and proportion of materials.Moreover comparing products of synthesized by two methods througth analyzing. The influence of the irradiation reaction time ,the quantities of urea and copper chloride and catalyst on the yield of copper phthalocyanine were investigated in microwave irradiation . we acquired the best proportion that is molbenzoic anhydrid:molurea:molCuCL=1:5:0.21 ,and ammonium molybolenum is equal to 3wt% of benzoic anhydride . For classical method ,reaction time is 2 hours and reaction temperature is located 210℃to220℃,the yield is best .under the selected same ratio of reactants ,the quality of product of synthesized by microwave irradiation method is better than that of conventional heating means,and the yield of microwave irradiation method was high than that of conventional heating means,and pollute of microwave is less than irradiation method conventional heating means.X-ray powder diffraction proved ,the products of two methods were mainly of βtype ,which was turned to αtype after being refined by concentrated sulfuric acid. Keyword:copper;phthalocyanine;microwave;irradiation;synthesis;benzoic anhydride;urea;CuCl; ammonium mo
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