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研究生:鄧瑾涵
研究生(外文):Jin-Han Deng
論文名稱:甘油與正丁醇連續反應之實驗研究
論文名稱(外文):Studies on Continuous Reaction of Glycerol and n-Butanol
指導教授:張志雄張志雄引用關係
指導教授(外文):Jyh-Shyong Chang
口試委員:張志雄
口試委員(外文):Jyh-Shyong Chang
口試日期:2017-07-21
學位類別:碩士
校院名稱:大同大學
系所名稱:化學工程研究所
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2017
畢業學年度:105
語文別:中文
論文頁數:72
中文關鍵詞:正丁醇連續反應酸觸媒甘油
外文關鍵詞:glyceroln-butanolcontinuous reactionacid catalyst
相關次數:
  • 被引用被引用:0
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  • 下載下載:6
  • 收藏至我的研究室書目清單書目收藏:0
本研究使用固體酸觸媒進行甘油與正丁醇之高壓與高溫連續式脫水反應,目的為連續產出且穩定的產物,因此需要穩定性高之觸媒與反應設備。由於備壓閥內部有個O型環,此環為穩定壓力之重要元件,若有雜質或粉末附著在上面,備壓閥會無法定壓,為了達到穩定產出之目標,固體酸觸媒必須為顆粒且通過高速轉軸時,不會被分解成粉末,本研究提供一種酸性觸媒顆粒的製備方法,其特徵具高熱穩定與長效用於一種酸催化反應。其製備方法包括:(a)使用一固體酸觸媒粉末具最佳的活性與穩定性,係經過一反應測試篩選出;(b)使用一醣類水溶液,該醣類水溶液內含:葡萄糖:4-羥基苯磺酸:水適當的重量比例;(c)該固體酸觸媒粉末與該醣類水溶液以適當重量比例下混合,在溫度60-90℃攪拌4-6小時,使形成一黑色膠狀體,該黑色之膠狀體在80℃經8-16小時烘乾可得黑色鬆軟固体;(d)將該黑色鬆軟固體置於一高壓釜內以氮氣持壓在一定溫度壓力下,維持30-60分鐘後排放出氣體,在2-4小時內重覆4至6次循環氮氣加壓、排氣、減壓步驟;(e)轉化該黑色鬆軟固体形成一堅硬塊狀物在一定的溫度壓力下維持4-6小時;(f)粉碎篩選該堅硬塊狀物可得適當大小之酸性觸媒顆粒,此顆粒酸觸媒在連續式反應進行88小時,甘油轉化率仍達64.02%。
The objective of this experimental study was to build a continuous reaction system for carrying out the dehydration reactions between glycerol and n-butanol (NB) operated steadily at high temperature and pressure. To achieve the objective, a solid catalyst pellet stirred by a high speed impeller shall not decompose into powders to make O-ring of the back-pressure regulator malfunction. If the O-ring of the back-pressure regulator cannot work properly, the reactor will lost it pressure and a steady operation of the continuous process cannot be maintained. A preparation method of high catalytic performance acid catalyst pellets was invented. This invention relates to a method for preparing an acid catalyst pellet with high thermo-stability and long life for acid catalysis reactions. The method includes: a) using a solid acid catalyst powder with an optimum activity and stability screening from a reaction test; b) using a saccharide solution wherein containing glucose, 4- hydroxyl- benzene sulfonic acid, water with a suitable weight ratio; c) mixing the solid acid catalyst powder and the saccharide solution with a suitable weight ratio, agitating the mixed solution at 60-90℃for 4-6h to form a black gel, putting the black gel into an oven at 80℃for 8-16h to obtain a soft solid; d) putting the soft solid into an autoclave keeping the temperature at a suitable temperature and pressure with nitrogen for 30-60 minutes, then releasing the gas to reduce the pressure of the autoclave, repeating the pressurization, gas release, depressurization steps for 4-6 cycle times during 2-4h ; e) transforming the soft solid into a hard lump matter by using nitrogen to keep the autoclave at a suitable temperature and pressure for 4-6h; and f) crushing the hard lump matter to obtain the acid catalyst pellet. The obtained solid catalyst pellets were performed for 88 hours and a high conversion of glycerol (64.02%) was still achieved.
中文摘要 I
Abstract I
目錄 II
圖目錄 VI
表目錄 VIII
第一章 緒論 1
1.1前言 1
1.2 文獻回顧 4
1.3 研究動機 7
第二章 實驗 8
2.1實驗藥品與觸媒介紹 8
2.2實驗步驟 9
2.2.1批式反應器 9
2.2.2連續式反應器 12
2.3產物之分析 20
2.3.1定性分析 21
2.3.2定量分析 27
第三章 結果與討論 30
3.1甘油與正丁醇反應之實驗範例 30
3.2實驗變因對甘油與正丁醇反應之影響 32
3.2.1實驗之操作變因 32
3.2.2轉化率及產率定義 33
3.2.3各觸媒對甘油與正丁醇反應之影響 35
3.2.4自製顆粒觸媒對甘油與正丁醇反應之影響 35
3.2.4.1顆粒觸媒製備 45
3.2.4.2顆粒觸媒對甘油與正丁醇反應之影響 46
3.4觸媒之性質檢驗 58
第四章 結論 61
參考文獻 63
附錄 66
(附錄一) 66
(附錄二) 72
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