摘要:本论文研究的新点是,以乙腈为溶剂,不经分水,使原料季戊四醇和苯甲醛溶解在均相中反应,产物在冷溶液中折出,大大简化了后处理。研究表明, 季戊四醇双缩苯甲醛的最佳工艺条件为:以氨基磺酸为催化剂,用量0.8g;反应时间3h;季戊四醇:苯甲醛=1:2.4,在此条件下,产物收率可达80.3%。产物结构通过红外光谱、核磁共振光谱进行了表征。43670
毕业论文关键词:季戊四醇;苯甲醛;双缩;乙腈;氨基磺酸
Synthesis of Pentaerythritol double benzaldehyde
Abstract: The new point of this paper is to acetonitrile as the solvent, without separation water treatment, the raw material pentaerythritol and benzaldehyde were dissolved in a homogeneous solution and the reaction product will precipitate in cold solution .All of this can greatly simplify the post-processing. Experiments show that the optimum conditions of the synthesis: the sulfamic acid as catalyst, the amount of 0.8g; reaction time 3h; pentaerythritol: benzaldehyde = 1: 2.4. Under these conditions, the yield can up to 80.3%.Condensation product structure by IR specttum and HNMR to characterize.
Key Words: Pentaerythritol; benzaldehyde; condensation; acetonitrile; sulfamic acid
目录
1、前言 1
1.1 开题依据 1
1.2. 季戊四醇缩醛(酮)的研究状况 2
1.2.1以硫酸为催化剂进行双缩 2
1.2.2以对甲苯磺酸为催化剂,环己烷为带水剂进行双缩 2
1.2.3以对甲苯磺酸为催化剂,苯为带水剂进行双缩 3
1.2.4以对甲苯磺酸为催化剂,环己烷为带水剂进行双缩 3
1.2.5以硫酸铝钾为催化剂,在微波辐射无溶剂条件下进行双缩 3
1.2.6以硫酸氢铵为催化剂,在微波照射无溶剂条件下进行双缩 3
1.2.7以杂多酸为催化剂,苯为带水剂情况下进行单缩 3
1.2.8杂以S2082-/Sn02-Si02固体超强酸为催化剂,苯为带水剂情况下双缩.........4
1.2.9以活性炭负载碘为催化剂,甲苯为带水剂情况下进行双缩 4
1.2.10以活性炭负载四氯化锡为催化剂,利用微波辐射法进行双缩 4
1.2.11以杂多酸-聚合物复合膜为催化剂,环己烷为带水剂进行双缩 5
1.2.12以稀土Ce4+复合钛基固体酸为催化剂,环己烷为带水剂进行双缩................5
1.2.13以活性炭负载磷钨酸为催化剂,以苯为溶剂进行缩合.....................................5
1.2.14以硫酸锆-硅胶为催化剂,利用微波辐射法进行双缩…………………………6
1.2.15以硫酸铝为催化剂,在微波辐射无溶剂情况下进行双缩……………………..6
1.2.16以SO42-/TiO2-SnO2固体超强酸为催化剂,无溶剂条件下进行双缩……….6
1.2.17以硫酸氢钾为催化剂,无溶剂微波辐射条件下进行双缩……………………..7
1.2.18以脱铝超稳Y沸石(简称DUSY)为催化剂,有溶剂条件下进行双缩………..7
1.2.19以可膨胀石墨为催化剂,甲苯为脱水剂进行缩合……………………………..7