奥克立林的合成工艺研究

摘要奥克立林是水溶性广谱紫外线吸收剂。本文探讨了奥克立林的合成工艺，主要进行了合成工艺路线选择和单因素工艺优化。得到的最佳工艺条件为：氰基乙酸与异辛醇以对甲苯磺酸为催化剂，以投料比为1:1.4在70 ℃反应5 h，纯度为97%，收率为92%，后处理得到氰乙酸异辛酯浓缩液，在其中加入二苯甲酮(投料比1.5:1) 和催化剂醋酸铵，溶剂正庚烷，发生Knoevenagel缩合反应，反应22 h，后处理制得浅黄色的奥克立林纯品，纯度99.5%，收率达86%。通过单因素实验得到合成最佳工艺条件，并通过1H-NMR和傅立叶红外光谱（IR)对中间体氰乙酸异辛酯和产物奥克立林进行了结构分析与表征。64296

毕业论文关键词：奥克立林；氰乙酸；异辛醇；Knoevenagel

1毕业设计说明书（论文）外文摘要

Title Study on the Process for Synthesis of Octocrilene

Abstract Octocrilene is a water soluble broad-spectrum UV absorber. This article focused on the synthesis of octocrilene, and tried to optimize the process. In this paper, the desirable conditions was investigated which adopted cyano acid and isooctanol(the reasonable ratio of 1:1.4) ,p-toluenesulfonic acid as catalyst, reacted at 70 ℃ for 5h, Then the products were given, which yield was 92%, the purity was 97%. In the post-processing, cyanide isooctyl esters was obtained, in which added benzophenone (feed ratio 1.5:1) and ammonium acetate catalyst, n-heptane as solvent, underwent the knoevenagel condensation reaction and reacted for 22h. After post-treatment , pure yellow sticky liquid was produced, which yield was 86% and purity was 99.5%.In order to optimize the reaction conditions, single factor experiment was employed. Meanwhile, the intermediate and target products were characterized through 1H NMR and IR spectra.

Keywords Octocrilene；Cyanoacetic acid ；iso-octyl alcohol；Knoevenagel

1引言 1

1.1紫外线吸收剂种类 2

1.2奥克立林 4

2研究内容 6

2.1 奥克立林的工艺研究 6

2.2研究手段 6

3 氰乙酸异辛酯的合成 6

3.1实验部分 6

3.2 单因素实验 8

3.3 结果讨论 10

3.4产物分析鉴定 11

4 2-氰基-3,3-二苯基丙烯酸异辛酯的合成 12

4.1 实验内容 12

4.2 单因素实验 14

4.3 结果讨论 16

4.4 产物分析鉴定 17

结论 20

致谢 21

参考文献 22

1引言

紫外线是在太阳光谱中波长为200 nm-400 nm部分的射线，大气中臭氧层阻碍了太阳光中99 %的紫外线辐射，是人类生活的天然屏障，1985年首次报道南极臭氧空洞以来，臭氧损耗成为全球性的环境问题之一。由此带来的紫外线辐射量激增产生的一系列问题也备受关注。随着紫外线辐射强度不断增加，并且呈现短波化的倾向，使达到地表的紫外线能量增加，给人类（包括生物界）的生存带来了严重的影响和危害。紫外线是引起皮肤晒伤并产生红斑的主要原因，它能对皮肤的表皮层直接损伤真皮层，破坏纤维组织，使皮肤老化，导致皮肤长期受损，甚至导致皮肤。此外，紫外线还能使高分子材料迅速发生老化，导致其外观、机械性能和电性能等显著恶化[1]。奥克立林的合成工艺研究:http://www.751com.cn/yixue/lunwen_71382.html