固体酸催化甲苯与苯酐合成2-甲基蒽醌反应研究.pdfVIP

固体酸催化甲苯与苯酐合成2-甲基蒽醌反应研究 ∗ 刘玉芝 王桂荣 王延吉 赵新强 （河北工业大学化工学院，天津，300130 ） 摘要：2- 甲基蒽醌是重要的有机合成中间体。工业上2- 甲基蒽醌生产常采用苯酐法。本文考察了不同 固体酸催化剂对甲苯与苯酐酰基化反应合成2- 甲基蒽醌的催化活性，筛选出合适的催化剂为H β沸石。当 催化剂焙烧温度550℃，催化剂用量为反应物的4.5% ，n(甲苯)：n （苯酐）=16:1，反应温度210 ℃，反应 时间5h，2- 甲基蒽醌收率可达20.2% 。对催化剂进行NH3-TPD 和Py-IR 表征，表明450 ℃、550℃焙烧的Hβ 沸石的弱酸及中强酸量几乎不变；450 ℃、550℃和650℃焙烧的Hβ沸石的L 酸中心与B 酸中心量之比大 于2, 焙烧温度增加，L/B 变化不太大。 关键词：2-甲基蒽醌；固体酸催化剂；Friedel-Crafts 酰基化反应 中图分类号：TQ 028.8 文献标识码：A Study on synthesis of 2-methyl anthraquinone from methylbenzene and phthalic anhydride over solid acid catalysts LIU Yuzhi WANG Guirong ZHAO Xinqiang , WANG Yanji (School of Chemical Engineering and Technology,Hebei University of Technology,Tianjin 300130,China) Abstract: 2-methyl anthraquinone is an important organic synthetic intermediate. The traditional method of the synthesis of 2-methyl anthraquinone is phthalic anhydride process. In this paper, the catalytic activity of several solid catalysts for the acylation reaction of methylbenzene and phthalic anhydride was examined, and the results showed that the better catalyst was Hβ zeolite. The optimal conditions are as follow: calcinatination temperature 550℃, mass fraction of catalyst 4.5%, n(methylbenzene): n(phthalic anhydride)=16:1, reaction temperature 210 ℃, reaction time 5h. Under the conditions, the yield of 2-methyl anthraquinone was 20.2%.The NH3-TPD and Py-IR characterization showed that the acid amount of Hβ zeolite at 450 and 550 ℃ calcination were almost identically, and the L/B of Hβ zeolite at 450 ℃, 550℃ and 650 ℃calcination were all greater than 2. Key words ：2-methyl anthraquinone ; Solid acid catalysts; Friedel-Crafts acylation 引 言 2- 甲基蒽醌是一种重要的蒽醌系染料中间体，主要用于合成有机中间体 1-硝基-2- 甲基 ∗基金项目：河北省自然科学基金资助项目（B2