萝藦科三种能源植物脂溶性成分提取与转化利用研究
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摘要
近年来随着温室气体排放的增加和原油价格的高涨,世界许多国家开始高度重视发展生物燃料,将其视为解决环境问题和能源问题的重要途径。人们普遍认为以生物质能,尤其是以能源植物作为原料来发展生物燃料是较为理想的选择。我国是世界上植物资源最为丰富的国家之一,拥有极其丰富的具有开发生物燃料潜在价值的能源植物资源,筛选、开发、可持续地利用能源植物资源发展生物燃料,是我国发展新兴能源产业的需要,也是调整能源结构、增加农业收入的需要,对于改善生态环境、保障能源供给安全具有重要意义。
本文筛选了我国北方常见的三种萝藦科植物(萝藦Metaplexis japonica (Thunb.) Makino、杠柳Periploca sepium Bunge、地梢瓜Cynanchum thesioides (Freyn) K.Schum作为研究对象,以石油醚为溶剂,分析了不同提取方法对三种能源植物地上营养体中脂溶性成分提取得率的影响,优化了提取工艺条件,检测了脂溶性提取物的主要成分；着重探究了杠柳Periploca sepium Bunge地上营养体水分和脂溶性成分含量的变化趋势,分析了杠柳Periploca sepium Bunge脂溶性成分(油脂)的理化性质并研究了其转化为生物液体燃料(生物柴油)的工艺流程,测定了杠柳Periploca sepium Bunge和萝藦Metaplexis japonica (Thunb.) Makino综纤维素和木质素含量。
主要研究结果如下：
(1)考察了超声波辅助提取法、闪式提取法对植物目的成分的提取工艺。在单因素试验的基础上,超声波辅助提取萝藦Metaplexis japonica (Thunb.) Makino脂溶性成分的优化工艺条件为超声波功率480W,提取时间52min,料液比1：12(g/mL),萝藦Metaplexis japonica (Thunb.) Makino脂溶性成分提取得率可达到8.4±0.13%；闪式提取法提取地梢瓜Cynanchum thesioides (Freyn) K.Schum脂溶性成分的优化工艺条件为提取电压145V,提取时间4min,料液比1：14(g/mL),地梢瓜Cynanchum thesioides (Freyn) K.Schum脂溶性成分提取得率可达到7.25±0.18%；超声波辅助提取杠柳Periploca sepium Bunge脂溶性成分的优化工艺条件为提取时间70min,超声波功率730W,料液比1：10(g/mL),杠柳Periploca sepium Bunge脂溶性成分的提取得率可达到6.14±0.28%。
(2)经过气相色谱的检测,萝藦Metaplexis japonica (Thunb.) Makino植物体脂溶性提取物的成分主要为棕榈酸、亚油酸、亚麻酸、硬脂酸和烃类等；地梢瓜Cynanchum thesioides (Freyn) K.Schum植物体脂溶性提取物的成分主要为棕榈酸、亚麻酸、硬脂酸、油酸和烃类等；杠柳Periploca sepium Bunge植物体脂溶性提取物的成分主要为亚油酸、棕榈酸和碳氢化合物等,可以作为制备生物液体燃料的原料。
(3)杠柳Periploca sepium Bunge植物体脂溶性成分和水分的含量与季节和气候有密切关系,根据脂溶性成分和水分含量变化趋势,采收杠柳Periploca sepium Bunge的适宜时间为8—9月份。
(4)通过对酸值、皂化值、过氧化值、碘价、相对密度、折光率、水分和杂质的测定,杠柳Periploca sepium Bunge油脂的各项理化性质指标均在正常范围之内。
(5)以杠柳Periploca sepium Bunge油脂为原料,通过使用两步法制备脂肪酸甲酯(生物柴油),运用响应面分析法得到制备生物柴油的最优工艺条件：反应温度为60℃,磁力搅拌器转速为300r/min,反应时间为98min,醇油摩尔比为7：1,催化剂用量为1.1%。在此条件下,实际转化率可达到90.78±2.62%。通过两步法获得的脂肪酸甲酯总转化率为92.59%。气相色谱法检测杠柳Periploca sepium Bunge油脂制备的脂肪酸甲酯主要成分为：亚油酸甲酯,棕榈酸甲酯,和少量的亚麻酸甲酯,油酸甲酯等。制备的脂肪酸甲酯(生物柴油)基本符合国家标准。通过精制纯化,副产物甘油的收率能达到预计值的40%,纯度可以达到90%左右。
(6)杠柳Periploca sepium Bunge综纤维素和木质素的含量分别为68.7%、13.1%,合计占总质量的81.8%；萝藦Metaplexis japonica (Thunb.)Makino综纤维素和木质素的含量分别为55.8%、4.9%,合计占总质量的60.7%。
(7)基于能源植物利用现状和本文研究结果,从加强科学研究、开展综合管理、构建法律保障体系、完善政策体系、合理配置资源等方面提出我国能源植物资源可持续发展利用的建议。
With the increase in greenhouse gas emissions and the rise in crude oil price in recent years, many countries have attached great importance to the development of bio-fuels and adopted it as the vital way to solve environmental and energy problems. It is widely considered that biomass energy, especially energy plants is the ideal source for the development of bio-fuels. China is one of the countries with the most abundant energy plant resources in the world that have the potential to develop bio-fuels. The screening, exploration and sustainable use of energy plant resources is adopted to develop the bio-fuels. It is the need of promoting new energy industry, adjusting energy structure and increasing agricultural income. It also has the vital implication for improving the ecological environment and safeguarding the security of the energy supply.
Three common Asclepiadaceae plant species(Metaplexis japonica (Thunb.) Makino, Periploca sepium Bunge and Cynanchum thesioides (Freyn) K.Schum) in the North China were studied in this paper. The author compared the effects of three different extraction methods on the extraction rate of fat-soluble components, optimized the extraction conditions, and detected the main components of fat-soluble extracts. In addition, the author explored the content change of water and fat-soluble components in Periploca sepium Bunge, analyzed the physicochemical properties of fat-soluble ingredients. The author also studied the process of conversing this oil to bio-liquid fuel, measured the contents of holocellulose and lignin in Periploca sepium Bunge and Metaplexis japonica (Thunb.) Makino.
The main study results are shown as follows:
(1)The methods of ultrasonic assisted extraction and flash-extractor extraction were adopted to study the target components in this paper. Based on the single-factor experiments, the results showed that the optimum conditions of ultrasonic assisted extraction for fat-soluble components from Metaplexis japonica (Thunb.) Makino were:ultrasonic frequency:20kHz, ultrasonic power:480W, ultrasonic assisted extraction time:52min, material-solvent ratio:1:12g/mL. On these conditions, the actual extraction yield was8.4±0.13%. The optimum conditions of flash-extractor extraction for fat-soluble components from Cynanchum thesioides (Freyn) K.Schum were:the voltage of extraction:145V, extraction time:4min, material-solvent ratio:1:14g/mL. On these conditions, the actual extraction rate was7.25±0.18%. The optimum conditions of ultrasound-assisted extraction for fat-soluble components from Periploca sepium Bunge were:Ultrasonic frequency:20kHz, ultrasonic power:730W, ultrasonic assisted extraction time:70min, material-solvent ratio:1:10g/mL, On these conditions, the actual extraction yield was6.14±0.28%.
(2) Through the detection of the fat-soluble components using the gas chromatography, the results showed that they were mainly composed of palmitic acid, linoleic acid, stearic acid and hydrocarbons in M.japonica, palmitic acid, linoleic acid, stearic acid, oleic acid and hydrocarbons in C. thesioides, linoleic acid, palmitic acid, hydrocarbons in P. sepium. These fat-soluble components can be used as the raw materials for making biological fluid fuel.
(3) The contents of water and fat-soluble components in the plant body of Periploca sepium Bunge are closely related to the season and climate. According to the changing trend of the above components, Periploca sepium Bunge should be timely harvested in August and September.
(4) The physicochemical characteristics of oil in Periploca sepium Bunge have been measured, including acid value, saponification value, peroxide value, iodine value, relative density, refractive index, moisture and impurities., The result showed that the values of the above indicators fell within the normal range.
(5) After biodiesel was prepared from Periploca sepium Bunge oil by two steps, response surface analysis methodology (RSM) was employed to optimize the process conditions:the reaction temperature was60℃, magnetic stirrer speed was300r/min, the reaction time was98min, methanol-oil molar ratio was7:1, catalyst amount was1.1%. On this condition, the actual conversion rate reached90.78%; According to the detection by gas chromatography, the main components of fatty acid methyl ester were methyl linoleate, methyl palmitate, methyl linolenate and a small amount of methyl oleate. After the purification, the yield of the by-product glycerin reached40%of the expected value and the purity was up to90%or so.
(6) The contents of holocellulose and lignin in Periploca sepium Bunge was respectively68.7%and13.1%, totally accounting for81.8%of the total weight. Besides, the contents of holocellulose and lignin in Metaplexis japonica (Thunb.) Makino was respectively55.8%and4.9%, totally accounting for60.78%of the total weight.
(7) Based on the utilization status of energy plants and the research in this paper, the author proposed the suggestion about the sustainable use of energy plant resources in the aspects of the scientific research, the comprehensive management, the construction of legal systems, the improvement of policy systems, and the reasonable allocation of resources.
本文筛选了我国北方常见的三种萝藦科植物(萝藦Metaplexis japonica (Thunb.) Makino、杠柳Periploca sepium Bunge、地梢瓜Cynanchum thesioides (Freyn) K.Schum作为研究对象,以石油醚为溶剂,分析了不同提取方法对三种能源植物地上营养体中脂溶性成分提取得率的影响,优化了提取工艺条件,检测了脂溶性提取物的主要成分；着重探究了杠柳Periploca sepium Bunge地上营养体水分和脂溶性成分含量的变化趋势,分析了杠柳Periploca sepium Bunge脂溶性成分(油脂)的理化性质并研究了其转化为生物液体燃料(生物柴油)的工艺流程,测定了杠柳Periploca sepium Bunge和萝藦Metaplexis japonica (Thunb.) Makino综纤维素和木质素含量。
主要研究结果如下：
(1)考察了超声波辅助提取法、闪式提取法对植物目的成分的提取工艺。在单因素试验的基础上,超声波辅助提取萝藦Metaplexis japonica (Thunb.) Makino脂溶性成分的优化工艺条件为超声波功率480W,提取时间52min,料液比1：12(g/mL),萝藦Metaplexis japonica (Thunb.) Makino脂溶性成分提取得率可达到8.4±0.13%；闪式提取法提取地梢瓜Cynanchum thesioides (Freyn) K.Schum脂溶性成分的优化工艺条件为提取电压145V,提取时间4min,料液比1：14(g/mL),地梢瓜Cynanchum thesioides (Freyn) K.Schum脂溶性成分提取得率可达到7.25±0.18%；超声波辅助提取杠柳Periploca sepium Bunge脂溶性成分的优化工艺条件为提取时间70min,超声波功率730W,料液比1：10(g/mL),杠柳Periploca sepium Bunge脂溶性成分的提取得率可达到6.14±0.28%。
(2)经过气相色谱的检测,萝藦Metaplexis japonica (Thunb.) Makino植物体脂溶性提取物的成分主要为棕榈酸、亚油酸、亚麻酸、硬脂酸和烃类等；地梢瓜Cynanchum thesioides (Freyn) K.Schum植物体脂溶性提取物的成分主要为棕榈酸、亚麻酸、硬脂酸、油酸和烃类等；杠柳Periploca sepium Bunge植物体脂溶性提取物的成分主要为亚油酸、棕榈酸和碳氢化合物等,可以作为制备生物液体燃料的原料。
(3)杠柳Periploca sepium Bunge植物体脂溶性成分和水分的含量与季节和气候有密切关系,根据脂溶性成分和水分含量变化趋势,采收杠柳Periploca sepium Bunge的适宜时间为8—9月份。
(4)通过对酸值、皂化值、过氧化值、碘价、相对密度、折光率、水分和杂质的测定,杠柳Periploca sepium Bunge油脂的各项理化性质指标均在正常范围之内。
(5)以杠柳Periploca sepium Bunge油脂为原料,通过使用两步法制备脂肪酸甲酯(生物柴油),运用响应面分析法得到制备生物柴油的最优工艺条件：反应温度为60℃,磁力搅拌器转速为300r/min,反应时间为98min,醇油摩尔比为7：1,催化剂用量为1.1%。在此条件下,实际转化率可达到90.78±2.62%。通过两步法获得的脂肪酸甲酯总转化率为92.59%。气相色谱法检测杠柳Periploca sepium Bunge油脂制备的脂肪酸甲酯主要成分为：亚油酸甲酯,棕榈酸甲酯,和少量的亚麻酸甲酯,油酸甲酯等。制备的脂肪酸甲酯(生物柴油)基本符合国家标准。通过精制纯化,副产物甘油的收率能达到预计值的40%,纯度可以达到90%左右。
(6)杠柳Periploca sepium Bunge综纤维素和木质素的含量分别为68.7%、13.1%,合计占总质量的81.8%；萝藦Metaplexis japonica (Thunb.)Makino综纤维素和木质素的含量分别为55.8%、4.9%,合计占总质量的60.7%。
(7)基于能源植物利用现状和本文研究结果,从加强科学研究、开展综合管理、构建法律保障体系、完善政策体系、合理配置资源等方面提出我国能源植物资源可持续发展利用的建议。
With the increase in greenhouse gas emissions and the rise in crude oil price in recent years, many countries have attached great importance to the development of bio-fuels and adopted it as the vital way to solve environmental and energy problems. It is widely considered that biomass energy, especially energy plants is the ideal source for the development of bio-fuels. China is one of the countries with the most abundant energy plant resources in the world that have the potential to develop bio-fuels. The screening, exploration and sustainable use of energy plant resources is adopted to develop the bio-fuels. It is the need of promoting new energy industry, adjusting energy structure and increasing agricultural income. It also has the vital implication for improving the ecological environment and safeguarding the security of the energy supply.
Three common Asclepiadaceae plant species(Metaplexis japonica (Thunb.) Makino, Periploca sepium Bunge and Cynanchum thesioides (Freyn) K.Schum) in the North China were studied in this paper. The author compared the effects of three different extraction methods on the extraction rate of fat-soluble components, optimized the extraction conditions, and detected the main components of fat-soluble extracts. In addition, the author explored the content change of water and fat-soluble components in Periploca sepium Bunge, analyzed the physicochemical properties of fat-soluble ingredients. The author also studied the process of conversing this oil to bio-liquid fuel, measured the contents of holocellulose and lignin in Periploca sepium Bunge and Metaplexis japonica (Thunb.) Makino.
The main study results are shown as follows:
(1)The methods of ultrasonic assisted extraction and flash-extractor extraction were adopted to study the target components in this paper. Based on the single-factor experiments, the results showed that the optimum conditions of ultrasonic assisted extraction for fat-soluble components from Metaplexis japonica (Thunb.) Makino were:ultrasonic frequency:20kHz, ultrasonic power:480W, ultrasonic assisted extraction time:52min, material-solvent ratio:1:12g/mL. On these conditions, the actual extraction yield was8.4±0.13%. The optimum conditions of flash-extractor extraction for fat-soluble components from Cynanchum thesioides (Freyn) K.Schum were:the voltage of extraction:145V, extraction time:4min, material-solvent ratio:1:14g/mL. On these conditions, the actual extraction rate was7.25±0.18%. The optimum conditions of ultrasound-assisted extraction for fat-soluble components from Periploca sepium Bunge were:Ultrasonic frequency:20kHz, ultrasonic power:730W, ultrasonic assisted extraction time:70min, material-solvent ratio:1:10g/mL, On these conditions, the actual extraction yield was6.14±0.28%.
(2) Through the detection of the fat-soluble components using the gas chromatography, the results showed that they were mainly composed of palmitic acid, linoleic acid, stearic acid and hydrocarbons in M.japonica, palmitic acid, linoleic acid, stearic acid, oleic acid and hydrocarbons in C. thesioides, linoleic acid, palmitic acid, hydrocarbons in P. sepium. These fat-soluble components can be used as the raw materials for making biological fluid fuel.
(3) The contents of water and fat-soluble components in the plant body of Periploca sepium Bunge are closely related to the season and climate. According to the changing trend of the above components, Periploca sepium Bunge should be timely harvested in August and September.
(4) The physicochemical characteristics of oil in Periploca sepium Bunge have been measured, including acid value, saponification value, peroxide value, iodine value, relative density, refractive index, moisture and impurities., The result showed that the values of the above indicators fell within the normal range.
(5) After biodiesel was prepared from Periploca sepium Bunge oil by two steps, response surface analysis methodology (RSM) was employed to optimize the process conditions:the reaction temperature was60℃, magnetic stirrer speed was300r/min, the reaction time was98min, methanol-oil molar ratio was7:1, catalyst amount was1.1%. On this condition, the actual conversion rate reached90.78%; According to the detection by gas chromatography, the main components of fatty acid methyl ester were methyl linoleate, methyl palmitate, methyl linolenate and a small amount of methyl oleate. After the purification, the yield of the by-product glycerin reached40%of the expected value and the purity was up to90%or so.
(6) The contents of holocellulose and lignin in Periploca sepium Bunge was respectively68.7%and13.1%, totally accounting for81.8%of the total weight. Besides, the contents of holocellulose and lignin in Metaplexis japonica (Thunb.) Makino was respectively55.8%and4.9%, totally accounting for60.78%of the total weight.
(7) Based on the utilization status of energy plants and the research in this paper, the author proposed the suggestion about the sustainable use of energy plant resources in the aspects of the scientific research, the comprehensive management, the construction of legal systems, the improvement of policy systems, and the reasonable allocation of resources.
引文
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