水楊酸乙酯的催化合成研究

化工論文編號(hào):HG066  論文字?jǐn)?shù):12435,頁(yè)數(shù):25

目　　錄
 中文摘要…………………………………………………………………………Ⅰ
 英文摘要…………………………………………………………………………Ⅱ
 目錄………………………………………………………………………………Ⅲ
1.緒論……………………………………………………………………………1
 1.1 引言………………………………………………………………………1
 1.2 研究現(xiàn)狀…………………………………………………………………2
 1.3 前景展望…………………………………………………………………4
2.實(shí)驗(yàn)部分………………………………………………………………………5
 2.1 實(shí)驗(yàn)原理…………………………………………………………………5
 2.2 實(shí)驗(yàn)原料與儀器…………………………………………………………7
 2.3 實(shí)驗(yàn)方案  ………………………………………………………………8
3.結(jié)果與討論    ………………………………………………………………9
 3.1 常規(guī)加熱催化合成水楊酸乙酯的最優(yōu)化設(shè)……………………………9
 3.2 微波輻射合成水楊酸乙酯的最優(yōu)化設(shè)計(jì) ……………………………13
4.總結(jié)與展望 …………………………………………………………………18
 致謝  ……………………………………………………………………………19
參考文獻(xiàn)  ………………………………………………………………………20
 附錄  ……………………………………………………………………………22

摘 要：本論文采用正交試驗(yàn)法，對(duì)常規(guī)加熱和微波輻射的方法催化合成水楊酸乙酯進(jìn)行了研究。按照L16(44)正交表進(jìn)行實(shí)驗(yàn)，并綜合分析實(shí)驗(yàn)數(shù)據(jù)后，對(duì)兩種方法下合成水楊酸乙酯的條件進(jìn)行了最優(yōu)化設(shè)計(jì)。在常規(guī)方法下，通過(guò)考察酸醇比，攪拌速率，催化劑用量，反應(yīng)時(shí)間四個(gè)因素對(duì)酯化產(chǎn)率的不同影響，得出其最佳反應(yīng)條件為：酸醇比為1:9，攪拌速率150r/min，催化劑用量3.5mL，反應(yīng)時(shí)間7小時(shí)，在該條件下酯化產(chǎn)率為70.82%。在微波輻射的方法下，通過(guò)考察酸醇比，微波功率，催化劑用量和反應(yīng)時(shí)間四個(gè)因素對(duì)產(chǎn)率的不同影響，得出最佳合成條件為：酸醇比1:9，微波功率325W，催化劑用量3.0ml，反應(yīng)時(shí)間50分鐘，在該條件下進(jìn)行實(shí)驗(yàn)得到的產(chǎn)率為73.75%。相比于常規(guī)方法，微波輻射合成法具有反應(yīng)時(shí)間短，產(chǎn)率高，副產(chǎn)物少，后處理簡(jiǎn)單的優(yōu)點(diǎn)，是一種合成水楊酸乙酯的理想方法。

關(guān)鍵詞: 水楊酸乙酯；微波輻射；催化酯化；正交設(shè)計(jì)

Study on the Catalysis Synthesis of Ethyl Salicylate

Abstract : This paper has carried on the orthogonal testing method to the conventional method as well as the microwave radiation synthesis of ethyl salicylate. This experiment used L16 (44) orthogonal table to complete the study of the catalysis synthesis of ethyl salicylate, and analysis of the experimental data for the optimized design . It investigated the yield of ester by using different proportion of salicylic acid and ethyl, different mix blend velocity, different quantity of sulfuric acid volume and different reaction time. The result enunciation that the most suitable and proper reaction conditions of the conventional method is that: the proportion of salicylic acid and ethyl is 1:9(the amount of salicylic acid is 0.05mol),mix blend the velocity is 150r/min, the sulfuric acid volume is 3.5 mL, and reaction time is 7 hours, and the ester produces a rate of 70.82%. The result enunciation that the most suitable and proper reaction conditions of the microwave radiation method is that:the proportion of salicylic acid and ethyl is 1:9(the amount of salicylic acid is 0.05mol),the powder is 325W,the sulfuric acid volume is 3.0 mL, and reaction time is 50 min, and the ester produces a rate of 73.75%. By comparison, the result shows that when microwave radiation technology was used in esterification, we can get short reaction times ,high yields,less byproducts and much more convenient in the process of after-treatment.
Keywords: Ethyl  salicylate; Microwave  radiation; Catalytic  esterification;  Orthogonal design