甘草酸的清洁生产工艺研究
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摘要
本文采用膜分离技术对甘草酸的传统生产工艺进行了清洁生产改造,对甘草酸的检测、提取、分离进行了系统的研究,对分离膜选择、工作特性、清洗方法进行了全面的讨论。
1.建立了甘草酸的高效液相色谱检测方法,确定了色谱条件。标准曲线相关系数R2=0.999903,重复性实验标准偏差为0.3886,相对标准偏差为0.42%,准确度高,可靠性强。
2.对浸提甘草酸时各影响因素进行了研究,确定了工艺参数,实验条件下甘草酸的提取率为2.90%。
3.对甘草酸浸提液膜除杂、浓缩工艺进行了研究,讨论了不同分离膜对浸提液除杂、浓缩的效果,对于不同要求的产品确定了三套不同的膜处理工艺。一级膜工艺得到与传统工艺纯度相当的产品,得率为2.82%,比传统工艺有明显提高;二级膜工艺得到纯度为42.12%的产品,得率为2.75%,纯度和得率都比传统工艺有所提高;三级膜工艺得到纯度高达60.92%的产品,比传统工艺有较大提高,得率为2.63%,比传统工艺略有下降。三套工艺的硫酸消耗量分别为传统工艺的20.75%、18.07%、和16.21%,产生的废液量分别为传统工艺的9.53%、9.53%和8.82%,都大为减少。
4.对酸沉上清液膜处理回用工艺进行了研究。确定了电渗析前絮凝法回收带电性物质,降低电导率和硫酸根浓度的工艺条件;确定了上清液经絮凝剂处理后,电渗析脱盐工艺的工艺参数;确定了电渗析淡水浓缩用膜和工艺参数。
5.对实验中用到的无机膜和有机膜的清洗进行了研究,确定了配制化学清洗剂的方法和清洗时的工作条件。实验表明,使用复合清洗剂在实验条件下对被污染的膜进行清洗,能使其纯水通量较好地恢复到接近新膜的水平。
本研究通过使用分离膜对甘草酸浸提液进行除杂、浓缩,显著提高了产品的纯度和得率,大大降低了耗酸量,并通过脱盐、浓缩工艺使酸沉上清液获得了回用,通过喷雾干燥工艺回收了其他固形物成分。整套工艺不产生三废污染,从生产过程中控制污染的产生,进行源头治污,真正做到了清洁生产,符合循环经济的理念,响应了国家清洁生产促进法,是实施可持续发展战略的需要。
In this paper,membrane technology had been used to improve the traditional production technology of glycyrrhizic acid(GA).Researches had been done systematically about the checking,extraction and separation.A thorough discussion had been done about the choosing, work characteristics and cleanout method of membrane.
1.The HPLC analysis conditions of the glycyrrhizic acid was decided.The correlative coefficient R2=0.999903,standard deviation of the repetitive experiments was 0.3886, relative standard deviation was 0.42%.The method was exact and reliable.
2.The influence factors of GA extraction had been studied,and the technologic parameter had been decided.The rate of extraction was 2.90%.
3.Researches and discussions had been done about the impurity removal and concentration technology about the extraction liquid of GA by membranes. The yield of one-order-membrane technology was 2.81%,which was much better than that produced by the traditional technology. The purity of the GA produced by two-oder-membrane technology was 42.12%,the yield was 2.75%,both of which were better than that produced by the traditional technology. The purity of the GA produced by three -order-membrane technology was 60.92%,which was a significant advance from the traditional technology.The consumptions of the oil of vitriol were respectively 20.75%,18.07% and 16.21% of that in the traditional technology.The wastewater produced in three technologies above were respectively 9.53%、9.53% and 8.82% of that in the traditional technology.
4.Researches had been done about the relamation technology of the wastewater. The conditions of the flocculation before the electrodialysis technology,the technology parameters of electrodialysis, and the membrane and the technology parameters to the concentration of desalted water of electrodialysis were decided.
5. Researches had been done about the cleanout of inorganic membranes and organic membranes.The compounding recipe of chemical detergent and the work conditions were decided. Experiments showed that the flux of fresh water recovered approximately to that of the new membranes after purged in the experiment condition. Impurity was removed and the extracted liquid was concentrated by membrane.The purity and jield were heightened,The consumption of the oil of vitriol was dramatically reduced,and the wastewater was recycled after desalting and concentration,meanwhile the concentrated solution was reused through spray drying.There was no production of three types of wastes,pollution was controlled in the process and curbed from the source,clean production came true authentically.It accorded with the recycle economy tenet,in answer to the law of people’s republic of China on promoting clean production,was the demand of the sustainable development strategy.
1.建立了甘草酸的高效液相色谱检测方法,确定了色谱条件。标准曲线相关系数R2=0.999903,重复性实验标准偏差为0.3886,相对标准偏差为0.42%,准确度高,可靠性强。
2.对浸提甘草酸时各影响因素进行了研究,确定了工艺参数,实验条件下甘草酸的提取率为2.90%。
3.对甘草酸浸提液膜除杂、浓缩工艺进行了研究,讨论了不同分离膜对浸提液除杂、浓缩的效果,对于不同要求的产品确定了三套不同的膜处理工艺。一级膜工艺得到与传统工艺纯度相当的产品,得率为2.82%,比传统工艺有明显提高;二级膜工艺得到纯度为42.12%的产品,得率为2.75%,纯度和得率都比传统工艺有所提高;三级膜工艺得到纯度高达60.92%的产品,比传统工艺有较大提高,得率为2.63%,比传统工艺略有下降。三套工艺的硫酸消耗量分别为传统工艺的20.75%、18.07%、和16.21%,产生的废液量分别为传统工艺的9.53%、9.53%和8.82%,都大为减少。
4.对酸沉上清液膜处理回用工艺进行了研究。确定了电渗析前絮凝法回收带电性物质,降低电导率和硫酸根浓度的工艺条件;确定了上清液经絮凝剂处理后,电渗析脱盐工艺的工艺参数;确定了电渗析淡水浓缩用膜和工艺参数。
5.对实验中用到的无机膜和有机膜的清洗进行了研究,确定了配制化学清洗剂的方法和清洗时的工作条件。实验表明,使用复合清洗剂在实验条件下对被污染的膜进行清洗,能使其纯水通量较好地恢复到接近新膜的水平。
本研究通过使用分离膜对甘草酸浸提液进行除杂、浓缩,显著提高了产品的纯度和得率,大大降低了耗酸量,并通过脱盐、浓缩工艺使酸沉上清液获得了回用,通过喷雾干燥工艺回收了其他固形物成分。整套工艺不产生三废污染,从生产过程中控制污染的产生,进行源头治污,真正做到了清洁生产,符合循环经济的理念,响应了国家清洁生产促进法,是实施可持续发展战略的需要。
In this paper,membrane technology had been used to improve the traditional production technology of glycyrrhizic acid(GA).Researches had been done systematically about the checking,extraction and separation.A thorough discussion had been done about the choosing, work characteristics and cleanout method of membrane.
1.The HPLC analysis conditions of the glycyrrhizic acid was decided.The correlative coefficient R2=0.999903,standard deviation of the repetitive experiments was 0.3886, relative standard deviation was 0.42%.The method was exact and reliable.
2.The influence factors of GA extraction had been studied,and the technologic parameter had been decided.The rate of extraction was 2.90%.
3.Researches and discussions had been done about the impurity removal and concentration technology about the extraction liquid of GA by membranes. The yield of one-order-membrane technology was 2.81%,which was much better than that produced by the traditional technology. The purity of the GA produced by two-oder-membrane technology was 42.12%,the yield was 2.75%,both of which were better than that produced by the traditional technology. The purity of the GA produced by three -order-membrane technology was 60.92%,which was a significant advance from the traditional technology.The consumptions of the oil of vitriol were respectively 20.75%,18.07% and 16.21% of that in the traditional technology.The wastewater produced in three technologies above were respectively 9.53%、9.53% and 8.82% of that in the traditional technology.
4.Researches had been done about the relamation technology of the wastewater. The conditions of the flocculation before the electrodialysis technology,the technology parameters of electrodialysis, and the membrane and the technology parameters to the concentration of desalted water of electrodialysis were decided.
5. Researches had been done about the cleanout of inorganic membranes and organic membranes.The compounding recipe of chemical detergent and the work conditions were decided. Experiments showed that the flux of fresh water recovered approximately to that of the new membranes after purged in the experiment condition. Impurity was removed and the extracted liquid was concentrated by membrane.The purity and jield were heightened,The consumption of the oil of vitriol was dramatically reduced,and the wastewater was recycled after desalting and concentration,meanwhile the concentrated solution was reused through spray drying.There was no production of three types of wastes,pollution was controlled in the process and curbed from the source,clean production came true authentically.It accorded with the recycle economy tenet,in answer to the law of people’s republic of China on promoting clean production,was the demand of the sustainable development strategy.
引文
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