發(fā)布時間：2018-04-03 23:57

  本文選題：酒糟　切入點：磺化炭基固體酸　出處：《合肥工業(yè)大學(xué)》2017年碩士論文

【摘要】：在石油化工和精細(xì)化工中,酸催化劑占有非常重要的地位。液體酸具有較高的催化活性因而廣泛地應(yīng)用于工業(yè)生產(chǎn)中,但其缺點是污染環(huán)境、腐蝕設(shè)備、產(chǎn)物難純化和催化劑難循環(huán)利用等。為克服液體酸的缺點,人們把固體酸引入到酸催化中,但當(dāng)前研究的固體酸也存在制備成本高和催化活性低的不足。因此研究成本低廉且高效的生物炭固體酸催化劑成為近年來催化劑研究的熱點。本文以酒糟為原料,研究了酒糟炭基磺酸化固體酸和酒糟炭負(fù)載型磷鎢酸催化劑的制備方法,并利用 XRD、FT-IR、XPS、TG、31PMASNMR、NH3-TPD、N2 吸附-脫附、元素分析和酸量滴定對制備的催化劑的組成、結(jié)構(gòu)和表面酸性進(jìn)行表征;通過乙酸和正丁酯的酯化反應(yīng)為探針反應(yīng)對制備的催化劑的催化活性和穩(wěn)定性進(jìn)行檢測,并利用氣相色譜、紅外光譜和折光率來研究催化劑的選擇性;同時還研究了酒糟炭基磺酸化固體酸在乳酸丁酯合成中的應(yīng)用。主要結(jié)果如下:(1)通過響應(yīng)面試驗設(shè)計得出一步炭化磺化法制備酒糟炭基磺酸化固體酸的最優(yōu)制備條件:硫酸濃度為85 wt%、制備溫度為20℃和制備時間為1.4 h;在此條件下制備的催化劑,酸密度為1.73 mmol/g,在探針反應(yīng)中催化乙酸轉(zhuǎn)化率達(dá)到97.6 %;催化劑催化活性隨使用次數(shù)增加逐漸降低,可通過85 wt%硫酸進(jìn)行再生。催化劑對乳酸正丁酯的催化合成同樣具有較高的活性和選擇性。(2)以酒糟炭為載體,采用浸漬法制備了一系列負(fù)載型磷鎢酸催化劑。磷鎢酸的負(fù)載量為50 wt%時,催化劑的催化活性較好。催化劑的比表面積為415 m2/g,磷鎢酸以Keggin型結(jié)構(gòu)均勻的分散在酒糟炭表面和孔道內(nèi)。負(fù)載型磷鎢酸催化劑適宜的酯化反應(yīng)條件:催化劑用量為0.008 g/g,醇酸比為1.4,反應(yīng)時間為2.0 h。在此條件下,乙酸的轉(zhuǎn)化率為97.4%,重復(fù)使用5次,乙酸的轉(zhuǎn)化率仍達(dá)到91.3%。
[Abstract]:Acid catalyst plays an important role in petrochemical industry and fine chemical industry.Liquid acids are widely used in industrial production because of their high catalytic activity, but their shortcomings are pollution of the environment, corrosion of equipment, difficult purification of products and difficult to recycle the catalyst, etc.In order to overcome the shortcomings of liquid acids, solid acids are introduced into acid catalysis. However, the current research on solid acids also has the disadvantages of high preparation cost and low catalytic activity.Therefore, the research of low cost and high efficiency biocarboxylic acid catalysts has become a hot topic in recent years.In this paper, the preparation methods of solid carbon-based sulfonic acid and carbon-supported phosphotungstic acid catalyst for distiller's grains were studied, and the composition of the catalysts prepared by XRDX FT-IRT, XPST TGN 31PMASN MRN NH 3-TPDN N 2 adsorption and desorption, elemental analysis and acid titration were studied.The structure and surface acidity were characterized. The catalytic activity and stability of the prepared catalysts were determined by the esterification of acetic acid and n-butyl ester as probes, and the catalytic activity and stability of the prepared catalysts were determined by gas chromatography.The selectivity of the catalyst was studied by infrared spectroscopy and refraction, and the application of solid carbon-based sulfonic acid in the synthesis of butyl lactate was also studied.The main results are as follows: (1) the optimum conditions for the preparation of solid carbon-based sulfonic acid from distillers' grains by one step carbonization sulfonation method were obtained by response surface test: the concentration of sulfuric acid was 85 wt, the preparation temperature was 20 鈩，

本文編號：1707465