【作者】 韩枫；

【导师】 李稳宏；

【作者基本信息】 西北大学 ， 化学工程， 2008， 博士

【摘要】 黄姜中的有效成分皂素是生产合成甾体激素类等药物的主要中间体,目前工业上生产皂素采用的传统工艺不但提取率低,更重要的是会产生大量含酸高、胶质重、色素浓的酸性废水,对环境造成了极其严重的危害。针对以上生产上急需解决的现实问题,本课题重点旨在从源头上减少皂素生产过程中产生的高浓度废水及废渣,进行黄姜资源化综合利用,达到清洁生产以及提高经济效益的目的,为黄姜产业的发展提供新的思路和方法。研究重点之一是预分离淀粉再经水解、提取制备皂素新工艺的开发,通过试验得到了该过程优化的工艺路线和操作参数;在此基础上对预分淀粉和纤维素制备皂素的组合工艺进行了一定的研究;并以黄姜组织细胞理论为依据,对黄姜中皂素和淀粉、纤维素的结合规律和分离原理进行了分析和探讨。以小试研究为基础对预分离淀粉制备皂素的工艺进行了工业化应用放大研究,探讨了放大过程中的关键生产单元所遇到的难点问题。工业化放大结果与传统工艺相比:皂素收率增加8%,浓硫酸用量降低5%,浓盐酸用量降低18%,每吨新鲜黄姜可得90.06kg的淀粉;排放的废水量降低63.3%,化学耗氧量(CODCr)减少68.5%,色度减少59.6%;通过原材料消耗和产品效益分析,该工艺有较大的盈利空间。本研究成果达到了工业化生产的水平、既平衡治理三废的费用并可获得一定经济效益的目的。通过环境扫描电镜(SEM)、激光粒度分析仪、X-射线衍射扫描(XRD)、差示扫描量热分析(DSC)和红外光谱分析(IR)等手段分别对制备的黄姜淀粉和纤维素进行了性能表征和分析;测定了黄姜淀粉的中常见的营养元素、蛋白质、氨基酸、矿物质等,进行了营养价值评价,并对其进行了食品毒理学安全性评价。得到了以皂素废水废渣为原料制备有机肥以及四种农作物专用肥的工艺路线,产品各参数符合有机肥标准NY525-2002。该工艺不但减轻了治理环境污染的压力,而且具有一定的经济价值。为了最大限度减少酸水解量,完成了从黄姜中先采用溶剂提取薯蓣皂苷再水解制备皂素新工艺的研究。通过薯蓣皂苷提取环节六种不同方法进行对比和机理分析基础上,得到了最理想的提取工艺—磨浆-超声波法,并在单因素考察基础上,通过响应面分析的工程计算模型得到了的最佳工艺条件及拟合方程;并对得到产品进行了结构表征和确认。该工艺同传统提取工艺相比:皂素收率的提高率为25.1%;产品纯度高;盐酸用量降低90%以上,石油醚用量降低了60%以上。该工艺有更为明显的环境效益和社会效益,具有良好的工业化开发前景。为了减少废水的色度和资源化利用的目的,对黄姜中黄色素提取工艺进行了研究;重点对色泽鲜艳的油溶性色素进行了精制、鉴别和稳定性等系统研究;并对水溶性色素采用大孔吸附树脂进行精制,并得到了吸附过程的等温吸附曲线及模型、动力学模型和热力学参数,解释了该吸附过程。本研究对黄姜的资源化综合利用进行了系统和全面的研究,充分利用了黄姜植物资源,解决了目前黄姜产业高污染、高能耗、资源利用率少和生产效率低下的问题。具有较高的环境、经济和社会价值,以及广阔的应用前景。更多还原

【Abstract】 As the main active ingredient of D.zingiberensis, Diosgenin is the important intermediate for the synthesis of steroid hormone medicine. But, there are so many disadvantages in the traditional process of the diosgenin production, such as the low extraction rate of diosgenin and lots of wastewater. The diosgenin acidic wastewater causes significant damage to the surrounding environment.This study put the main emphasis on the methods and ways of comprehensive utilization of D.zingiberensis as resource materials, in order to reduce acidic waste water and waste slag generated radicaly in the process of diosgenin production, aims to increase the economic efficiency with by-products, and provide new ideas and methods for the development of D.zingiberensis industry.A new Pre-separation of Starch Process and optimization coditions were obtained, which through pre-separation starch, hydrolysis and extraction to produce diosgenin from D.zingiberensis. Meanwhile the separation process of cellulose from D.zingiberensis was discussed, and Pre-separation of Starch and Cellulose Process was obtained. Through histocytology and experiment courses, the separation and combination principle of starch, cellulose and diosgenin in the D.zingiberensis were analyzed and discussed.The industrialization of Pre-separation of Starch Process was studied. Compared with traditional process, the yield of diosgenin was increased by 8%, the consumption of hydrochloric acid and sulphuric acid reduced by 18% and 5% respectively, and 90.06 kg of starch was obtained from one ton of fresh D.zingiberensis. The discharge amount of wastewater decreased by 63.3%, COD declined by 68.5%, chroma of it reduced by 59.6%. The process has greater profit through the consumption of raw materials and products-benefit analysis.The research results reached the level of industrial production, and achieved the target of environmental pollution improvement and getting some profits.Physicochemical property of D.zingiberensis starch and cellulose were detected and analyzed through Scanning Electronic Microscope, Laser Particle Size Analyser, X-Ray Diffractometer,Differential Scanning Calorimetry and Infrared Spectrum Analysis. Through testing the proteins, amino acids, minerals of D.zingiberensis starch, its nutritive value was discussed, through toxicology experiments, its safety was measured.A new preparation method of organic fertilizer with waste-water and waste slag generated in the traditional production process of diosgenin was studied, and preparation methods of four crops special organic fertilizer also were obtained, all these products complied with the organic fertilizer standards NY525-2002. These methods can not only reduce environmental pollution, but also bring about certain economic benefits.In order to minimize acid waste-water generated in the production process of diosgenin, a new process of ethanol extracting and hydrochloric acid hydrolyzing was provided to extract diosgenin. Six different extracting methods were studied and compared, and the reaction mechanism was discussed. The grinding starch and ultrasonic extracting method was proved more efficient. By response surface methodology, the parameters of extraction process were optimized, the optimal process parameters and fitted regression equation were obtained. The molecular structure of the products were detected and determined. Compared with the traditional process, yield of diosgenin was raised by 25.1 percent, the consumption of hydrochloric acid reduced by 90%, and the consumption of petroleum benzine decreased by 60%, and the production was much purer. The method has some advantages such as higher efficiency, energy-saving and low pollution.In order to reduce chroma of waste-water generated in the production process of diosgenin and improve the level of comprehensive utilization of D.zingiberensis, extracting process of D. zingiberensis yellow pigment was studied. The research of refining, identification and stability of oil pigment were conducted. And the adsorption process of water pigment with macropore resin was studied, the absorption isotherm, dynamical equation and thermodynamic parameter of dsorption process were researched and discussed.A systematic and comprehensive study was made to have comprehensive utilization of D.zingiberensis, and solve the problem of high pollution and energy consumption, low availability of resources and production efficiencies in the current D.zingiberensis industry. It has a high environmental, economic and social benefits, and broad prospects.更多还原