【作者】 李静；

【导师】 周彩荣； 石晓华；

【作者基本信息】 郑州大学 ， 化学工艺， 2007， 硕士

【摘要】 肌醇广泛应用于医药、食品、饲料、日化等行业，是一种高附加值的精细化工原料。近年来该产品由于一些新用途的不断开发而成为国际市场上紧俏的化工商品之一。本文采用一种生产肌醇的新方法，在常压及高沸点溶剂多元醇存在下，以固体超强酸作催化剂，植酸水溶液经加热水解、过滤、结晶和烘干等工序，制备肌醇。由于催化剂自身的特性，肌醇可一次性结晶而获得较高质量的成品，从而简化了除杂、脱色、浓缩等工序。本文采用不同条件下制备的SO₄^2-／TiO₂型固体超强酸作为水解工业植酸的催化剂，运用4因素4水平的正交试验法筛选了植酸水解的工艺条件。结果表明不同因素对水解结果影响的大小为：催化剂型号＞甘油配比＞反应时间＞催化剂用量。水解工业品植酸的较佳工艺条件是：催化剂用Ti22，水解时间为21h，工业植酸和甘油的质量配比为3.5，催化剂用量为工业植酸质量的0.25％。同时考察了不同制备条件下得到的SO₄^2-／TiO₂型固体超强酸催化剂对植酸水解的影响，确定了SO₄^2-／TiO₂型固体超强酸催化剂制备过程中采用的硫酸溶液浓度为1.00mol／L，干燥温度为100℃，焙烧温度为500℃，焙烧时间为2h时。本文还对SO₄^2-／TiO₂型固体超强酸就表面酸强度、比表面积和热分析等方面进行了研究。根据本实验室前期研究出的结果，从废弃物水稻稻壳中成功地提取出了菲丁，菲丁的平均提取率为3.63％。本实验采用溶离的方法从菲丁中提取植酸。当把水解工业植酸的较佳工艺条件（水解转化率为72.35％）用于从废弃物稻壳中提取的植酸溶液水解时，植酸的水解转化率为62.98％。本文采用XRY-1C氧弹热量计、差示扫描量热法（DSC）和热重法（DTA-TGA）对肌醇进行了热分析研究。测得肌醇的标准摩尔燃烧焓为-2805.1kJ·mol^-1，并计算出肌醇的标准摩尔生成焓为-1270.94kJ·mol^-1。用DSC法测得肌醇了的熔程为225.37～231.92℃，熔化热为256.67J·g^-1，用DTA-TGA联合分析得到的肌醇分解温度在300℃以上。丰富了肌醇的有关热力学数据，为该产品的新工艺开发、设计和工业化生产提供了相关基础数据。更多还原

【Abstract】 Inositol is a fine chemical industry raw material, and has higher value-add. It has been widely applied to the industry of pharmaceutical, food, feed, as well as daily chemical matters, and so on.A new preparation technique of inositol was investigated from paddy hull in this paper. Putting high boiling polyhydric alcohol and certain quantity of solid super acid catalyst into an aqueous solution of phytic acid, in which the phytic acid was hydrolyzed at atmospheric pressure. Inositol was obtained after filtering, crystaling, drying hydroiyzing resultants. Due to the particularity of the catalyst, it was possibility that higher quality of inositol can be carried out with success during one-time crystallization. Because of the characteristic of catalyst, this process of hydroiyzing phytic acid was simplified during the technique of inositol, such as removing from impurities, decoloring, concentrating, and so on.The different SO₄^2-/TiO₂ solid super acids of which applied as the catalysts of hydroiyzing phytic acid were prepared. The reacting conditions were optimized by means of the Orthogonal Test Method （L16-4-4）. The experimental results showed that there were different effects of different factors on the phytic acid hydroiyzing reaction. The sequence of effect on the reaction result was given by the type of catalyst > proportion of glycerin > reaction time > usage of catalyst. The better technical conditions were acquired in which were the Ti22 type of catalyst, 3.5 the proportion of glycerin to phytic acid, the reaction time of 21h, and the dosage of catalyst was 0.25% of the quality of phytic acid, respectively. The effects of different preparation method of SO₄^2-/ TiO₂ solid super acids on the phytic acid hydroiyzing reaction were investigated, and the best preparation conditions were made sure in which the concentration of the spirit of sulphur was 1.00 mol/L, the temperature of dryness was 100℃, the temperature of calcinations was 500℃, the time of calcinations was 2h, respectively. The surface acid strength, specific surface area and thermal analysis were studied on SO₄^2-/TiO₂ solid super acid.On the basic of the results extracted phytin from paddy hull at our laboratory previously, phytic acid was extracted from phytin by dissolving method. According to given the better technical conditions of industry phytic acid hydrolyzating reaction in this paper, the phytic acid extracted from paddy hull was hydrolyzed, and the conversion rate was 62.98%. It was lower than the hydrolyzating conversion 72.35% of which came from the industry phytic acid.The thermodynamics of inositol were determined by XRY-1C calorimeter, DSC and DTG-TGA, respectively. The combustion enthalpy and the formation enthalpy of inositol is -2805.1 kJ·mol^-1 and -1270.94 kJ·mol^-1 at the standard state. The melting range, the melting heat, and decomposition temperature is 225.37～231.92℃, 256.67 J·g^-1, 300℃for inositol, respectively. The necessary basic data of inositol are provided for the exploiting new synthesis method, engineering design and industrialized production.更多还原