毛竹叶总黄酮的分离研究及基于循环经济的毛竹产业链设计
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摘要
毛竹特产我国,是我国经济价值最高的竹种,广泛应用于社会生活的众多方面。但从总体上看,毛竹的综合利用技术尚处于起步阶段,毛竹产业还基本上处于粗放型经营的状态。循环经济以推进可持续发展为宗旨,以“减量化、再利用、再循环”为原则。因此,本课题根据循环经济的理念,首次提出了一条毛竹产业链。其中,“竹叶黄酮厂”是产业链中非常重要的一环。目前毛竹叶资源尚未得到较好地开发利用,为了实现毛竹叶黄酮的连续工业化生产,从而大规模地开发毛竹叶资源,本课题对毛竹叶总黄酮的提取分离工艺进行了研究,然后在此基础上对产业链中的“竹叶黄酮厂”进行了工艺流程的初步设计。主要内容包括:
1.运用循环经济的原则,模仿生态系统的物质流和能量流,首次提出了一条毛竹产业链,以毛竹资源的深加工为主线,构建了从毛竹林培育、鲜笋加工到毛竹全株利用的产业体系。该产业链主要包括笋竹两用林、笋制品厂、竹叶黄酮厂、竹材人造板厂、竹炭厂、手工厂和饲料厂等七个环节。七个环节之间通过废弃物的减量、再用和循环,以及能量的集成,以期实现产业链的低消耗、低排放。
2.为了较准确地测定毛竹叶提取物中的总黄酮含量,重点考察了NaNO_2-Al(NO_3)_3-NaOH显色法、紫外分光光度法和AlCl_3-(HAc-NaAc)显色法,发现以AlCl_3-(HAc-NaAc)显色法测定毛竹叶总黄酮含量比较好。
3.研究了毛竹叶总黄酮的浸取工艺,考察了浸取溶剂、固液比等条件对浸取效果的影响,得到了一条较好地浸取毛竹叶总黄酮的工艺路线。然后采用间歇萃取的方式对浸取物中的总黄酮进行了分离研究,考察了溶剂类型、萃取次数、萃取剂用量、原料液浓度等因素对萃取效果的影响,得到了间歇萃取分离毛竹叶总黄酮的合适的工艺条件。
4.针对现有脉冲萃取塔中脉冲发生器容易跑冒滴漏的现象,研制了一种新型的脉冲发生器。该新型脉冲发生器以磁力驱动旋转阀代替传统的机械旋转阀,解决了泄漏问题,而且只用两个脉冲罐就实现了同现有脉冲发生器(含有四个脉冲罐)同样的脉冲效果,从而简化了设备。然后以该新型脉冲发生器为基础,搭建了一套相应的脉冲填料萃取塔装置。
5.为实现毛竹叶总黄酮的连续化分离,促进毛竹叶资源的规模化利用,将所研制的脉冲填料萃取塔用于毛竹叶总黄酮的萃取分离研究,并且取得了较好的分离效果。首先考察了正丁醇-水体系在脉冲填料萃取塔(塔径25mm,有效填料高度0.70m)上的液泛特性,然后研究了脉冲速度、相比、流体总流量等因素对总黄酮萃取效果的影响。
Phyllostachys pubescens Mazel. (P. pubescens) is a local bamboo with prominent economic value in China. And the industry of P. pubescens has been of high-consumption and low-efficiency. So far, a product chain is proposed based on the strategy of circular economy to promote the sustainable development of P. pubescens industry. The total flavonoids extracted from P. pubescens leaves have remarkable bioactivity, such as anti-free radical, anti-oxidation, etc, and the correlative research has just been in the starting phase. In order to make use of the abundant leave resource more effectively, a process for extracting and separating total flavonoids from P. pubescens leaves is studied. The main contents are as follows:
1. Imitating material flows and energy flows of ecosystem, a product chain of P. pubescens is proposed based on the three principles of circular economy, i.e. reducing, reusing and recycling. The chain covers bamboo forest cultivation, utilization of shoot and the whole-bamboo use, and forms a multi-level product structure. The chain is composed of seven sections, namely the bamboo stand, the shoot plant, the flavonoids plant, the panel board plant, the charcoal plant, the handwork plant and the feed-processing plant. In the chain, special attention is paid to heat integration and water integration, and the closed cycles of resource and energy are approximately carried out.
2. To determine the content of total flavonoids in the extracts from P. pubescens more accurately, three colorimetric methods (NaNO_2-Al(NO_3)_3-NaOH colorimetry ultraviolet spectrophotometry, and AlCl_3-(HAc-NaAc) colorimetry) are compared. And a simple AlCl_3-(HAc-NaAc) colorimetry is proposed.
3. The influences of solvent and mass of leaves to volume of solvent on the leaching of total flavonoids from P. pubescens leaves are studied, and the suitable conditions are obtained. The crude leaching product is purified by the batch solvent extraction. In order to optimize the batch extraction process, the suitable extractant is chosen and the effects of feed concentration, ratio of solvent volume to feed volume and extraction times on the extraction yield and purity are investigated, respectively.
4. To solve the problem of poor seal existed in the traditional pulser, a new-style pulser is developed. With a magnetic drive rotary valve instead of the conventional mechanical rotary valve, and two pulsed pots instead of four in the traditional pulser, the new one is better sealed and simpler. Based on this new pulser, a pulsed packed extraction column (PPEC) is developed.
5. The PPEC with a diameter of 25mm and an effective packing height of 700mm is applied to implement the continuous extraction of the total flavonoids from the crude leaching products. The flooding characteristic of n-butanol-water system is studied, and the influences of pulsation intensity and ratio of solvent volume to feed volume on extraction performances are investigated.
1.运用循环经济的原则,模仿生态系统的物质流和能量流,首次提出了一条毛竹产业链,以毛竹资源的深加工为主线,构建了从毛竹林培育、鲜笋加工到毛竹全株利用的产业体系。该产业链主要包括笋竹两用林、笋制品厂、竹叶黄酮厂、竹材人造板厂、竹炭厂、手工厂和饲料厂等七个环节。七个环节之间通过废弃物的减量、再用和循环,以及能量的集成,以期实现产业链的低消耗、低排放。
2.为了较准确地测定毛竹叶提取物中的总黄酮含量,重点考察了NaNO_2-Al(NO_3)_3-NaOH显色法、紫外分光光度法和AlCl_3-(HAc-NaAc)显色法,发现以AlCl_3-(HAc-NaAc)显色法测定毛竹叶总黄酮含量比较好。
3.研究了毛竹叶总黄酮的浸取工艺,考察了浸取溶剂、固液比等条件对浸取效果的影响,得到了一条较好地浸取毛竹叶总黄酮的工艺路线。然后采用间歇萃取的方式对浸取物中的总黄酮进行了分离研究,考察了溶剂类型、萃取次数、萃取剂用量、原料液浓度等因素对萃取效果的影响,得到了间歇萃取分离毛竹叶总黄酮的合适的工艺条件。
4.针对现有脉冲萃取塔中脉冲发生器容易跑冒滴漏的现象,研制了一种新型的脉冲发生器。该新型脉冲发生器以磁力驱动旋转阀代替传统的机械旋转阀,解决了泄漏问题,而且只用两个脉冲罐就实现了同现有脉冲发生器(含有四个脉冲罐)同样的脉冲效果,从而简化了设备。然后以该新型脉冲发生器为基础,搭建了一套相应的脉冲填料萃取塔装置。
5.为实现毛竹叶总黄酮的连续化分离,促进毛竹叶资源的规模化利用,将所研制的脉冲填料萃取塔用于毛竹叶总黄酮的萃取分离研究,并且取得了较好的分离效果。首先考察了正丁醇-水体系在脉冲填料萃取塔(塔径25mm,有效填料高度0.70m)上的液泛特性,然后研究了脉冲速度、相比、流体总流量等因素对总黄酮萃取效果的影响。
Phyllostachys pubescens Mazel. (P. pubescens) is a local bamboo with prominent economic value in China. And the industry of P. pubescens has been of high-consumption and low-efficiency. So far, a product chain is proposed based on the strategy of circular economy to promote the sustainable development of P. pubescens industry. The total flavonoids extracted from P. pubescens leaves have remarkable bioactivity, such as anti-free radical, anti-oxidation, etc, and the correlative research has just been in the starting phase. In order to make use of the abundant leave resource more effectively, a process for extracting and separating total flavonoids from P. pubescens leaves is studied. The main contents are as follows:
1. Imitating material flows and energy flows of ecosystem, a product chain of P. pubescens is proposed based on the three principles of circular economy, i.e. reducing, reusing and recycling. The chain covers bamboo forest cultivation, utilization of shoot and the whole-bamboo use, and forms a multi-level product structure. The chain is composed of seven sections, namely the bamboo stand, the shoot plant, the flavonoids plant, the panel board plant, the charcoal plant, the handwork plant and the feed-processing plant. In the chain, special attention is paid to heat integration and water integration, and the closed cycles of resource and energy are approximately carried out.
2. To determine the content of total flavonoids in the extracts from P. pubescens more accurately, three colorimetric methods (NaNO_2-Al(NO_3)_3-NaOH colorimetry ultraviolet spectrophotometry, and AlCl_3-(HAc-NaAc) colorimetry) are compared. And a simple AlCl_3-(HAc-NaAc) colorimetry is proposed.
3. The influences of solvent and mass of leaves to volume of solvent on the leaching of total flavonoids from P. pubescens leaves are studied, and the suitable conditions are obtained. The crude leaching product is purified by the batch solvent extraction. In order to optimize the batch extraction process, the suitable extractant is chosen and the effects of feed concentration, ratio of solvent volume to feed volume and extraction times on the extraction yield and purity are investigated, respectively.
4. To solve the problem of poor seal existed in the traditional pulser, a new-style pulser is developed. With a magnetic drive rotary valve instead of the conventional mechanical rotary valve, and two pulsed pots instead of four in the traditional pulser, the new one is better sealed and simpler. Based on this new pulser, a pulsed packed extraction column (PPEC) is developed.
5. The PPEC with a diameter of 25mm and an effective packing height of 700mm is applied to implement the continuous extraction of the total flavonoids from the crude leaching products. The flooding characteristic of n-butanol-water system is studied, and the influences of pulsation intensity and ratio of solvent volume to feed volume on extraction performances are investigated.
引文
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