低品质米糠原位制备脂肪酸甲/乙酯研究及其综合利用设计
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摘要
随着世界能源危机和环境问题的加剧,寻找可再生新能源已成为各国战略发展的必然趋势。在这样的大背景下,从上世纪末至今,生物柴油受到了广泛的关注,且正以破竹之势蓬勃发展。此外,如何科学地、可持续发展地利用资源、保护环境也成为新世纪之初的重要议题和未来资源利用的大方向。
本论文基于上述的背景,针对目前生物柴油存在的问题,设计研究了一套利用低品质原料油制备生物柴油的方法,并对其中的废水、废渣进行了合理的利用,制得了高附加值的纳米碳酸钙产品。同时,我们将该方法改良应用于米糠原位提油制备生物柴油的研究。利用同步除水和酸碱逐步过渡两个关键技术,成功地将米糠提油和生物柴油的制备融为一体,缩短了工艺流程。该工艺以甲醇或乙醇为酯化/醇解剂,以石油醚为提油溶剂和反应介质,以硫酸为催化剂,在提油过程中实现米糠油中游离脂肪酸的原位酯化。在除水剂存在下,通过逐步加碱实现体系的酸碱过渡,从而使米糠油中的甘油酯醇解为生物柴油的主要成分脂肪酸甲酯或乙酯。该方法环境友好、具有一定的普适性,可应用于其它含油作物原位提油制备生物柴油。通过对提油过程、酯化过程和酯交换过程的考察,我们进一步设计并提出了米糠综合利用的工艺流程。初步的试验证实了该工艺的可行性,为米糠的综合利用探明了方向。
Under the pressure of energy and environment crisis, finding renewable environmentally friendly energy is becoming a great trend of the world. In this situation, bioengery such as fatty acid methyl ester (FAME) and fatty acid ethyl ester (FAEE) has attracted a lot of attention. FAME and FAEE have similar molecular structure and combustibility with the fossil diesel oil. They are typical renewable environmentally friendly energy, and usually called biodiesel. Besides, they could also be used as substitute of some traditional toxic organic solvent, because they have good solubility and resolvability. However, with the development of biodiesel industry, the problem of raw material has become a major constraint to the further development of this industry. Because the cost of the oil-containing material takes more than 70% cost of the biodiesel product, a lot of researches focus on the cheap raw materials. In another aspect, China produces more than 10,000,000 tons of rice bran annually and most of the rice bran is utilized unreasonably. As realized the problems of these two areas, we used low quality rice bran to produce FAME and FAEE in this dissertation, which is killing two birds with one stone. Based on the research, we made integrated strategies of rice bran utilization, too.
Firstly, we need to design a process which could produce FAME and FAEE from low quality feedstock oil. Traditionally, the typical method using low quality oil to produce FAME and FAEE is two-step process. The first step is an acid catalyzed process, which esterifies free fatty acids (FFAs), and the second step is an alkaline catalyzed process, which transesterifies the glycerides in the feedstock. However, the intermediate treatment process between esterification and transesterificaion processes is a tedious procedure including neutralization of acid catalyst, removal of water and impurities, evaporation of alcohol or settlement for phase-separation, et al. The tedious work not only wastes a lot of time, but also produces waste water which is unfriendly to the environment. In our work, we evolved a simple route for the production of FAME and FAEE, by using the mixture of soybean oil and oleic acid (OA) as feedstock to imitate low quality lipids with substantial FFAs content. The merit of our route is that the intermediate process could be eliminated based on our designed experimental apparatus, thus acid and alkaline catalyzed processes performed without intervals. The water in the reaction system was eliminated simultaneously when it was formed by introduction of CaO powder to Soxhlet apparatus. On considering the environmental character of the whole strategy, the waste water and CaO residue were used as raw materials to produce value-added nano-CaCO3 byproduct via carbonation method at room temperature. Based on our strategy, the production process of FAME and FAEE could be simplified and the production cost could be reduced. It was an economical route for FAME and FAEE production.
Secondly, based on the designed process, we studied the production of FAEE from low quality rice bran. The effects of solvent, acid and alkaline catalysts on the yield rate, esterification rate and transesterification rate were studied. 12.29% ( w FAEE / wrice?bran) of FAEE was obtained when absolute ethanol was used as solvent to extract rice bran oil. The esterification rate and transesterification rate reached 97.90 % and 82.78 %, respectively. With the aid of petroleum ether, the yield rate of FAEE could be improved to 15.50% ( w FAEE / wrice?bran), and the esterification rate and transesterification rate reached 98.89% and 85.94%. Moreover, we found that the petroleum ether could restrain saponification in the case of FAEE production.
Thirdly, we further studied the production of FAME from low quality rice bran. The oil extraction process and the effect of petroleum ether on the esterification and transesterification processes were investigated. Besides, the moister resistance of the system was investigated, too. The results approved that the designed process was feasible. It was different from FAEE that we found there was a synergistic effect between methanol and petroleum ether. Less methanol and acid catalyst could be used because of this effect. When 50 g of rice bran, 75 mL of absolute methanol, 150 mL of petroleum ether, 0.75 g of concentrated sulfuric acid and 0.71 g of sodium hydroxyl were used, 16.69% ( w FAME / wrice?bran) of FAME was obtained. The esterification rate and the transesterification rate reached 98.83% and 80.47%.
Finaly, on considering the environmental character of the whole strategy, we investigated the utilization of the waste water and CaO residue from FAME and FAEE production. In this chapter, value-added calcium carbonate (CaCO3) with micro/nanostructures was produced via carbonation method at ambient temperature. The results showed that the CaCO3 obtained was hydrophobic (contact angle, 111o) and had broccoli-like morphology. It was made up of many uniform nano-rods, and each rod was composed of smaller particles with diameters about 50 nm. The idea of wastes utilization could make the FAME/FAEE production process environmentally friendly, and the income of the produced CaCO3 could further compensate the cost of FAME/FAEE production.
The integrated utilization of rice bran is a promising project. As a result, at the end of the dissertation, we designed some technical flows for the further investigation of rice bran and hope it would be useful for the coming works.
本论文基于上述的背景,针对目前生物柴油存在的问题,设计研究了一套利用低品质原料油制备生物柴油的方法,并对其中的废水、废渣进行了合理的利用,制得了高附加值的纳米碳酸钙产品。同时,我们将该方法改良应用于米糠原位提油制备生物柴油的研究。利用同步除水和酸碱逐步过渡两个关键技术,成功地将米糠提油和生物柴油的制备融为一体,缩短了工艺流程。该工艺以甲醇或乙醇为酯化/醇解剂,以石油醚为提油溶剂和反应介质,以硫酸为催化剂,在提油过程中实现米糠油中游离脂肪酸的原位酯化。在除水剂存在下,通过逐步加碱实现体系的酸碱过渡,从而使米糠油中的甘油酯醇解为生物柴油的主要成分脂肪酸甲酯或乙酯。该方法环境友好、具有一定的普适性,可应用于其它含油作物原位提油制备生物柴油。通过对提油过程、酯化过程和酯交换过程的考察,我们进一步设计并提出了米糠综合利用的工艺流程。初步的试验证实了该工艺的可行性,为米糠的综合利用探明了方向。
Under the pressure of energy and environment crisis, finding renewable environmentally friendly energy is becoming a great trend of the world. In this situation, bioengery such as fatty acid methyl ester (FAME) and fatty acid ethyl ester (FAEE) has attracted a lot of attention. FAME and FAEE have similar molecular structure and combustibility with the fossil diesel oil. They are typical renewable environmentally friendly energy, and usually called biodiesel. Besides, they could also be used as substitute of some traditional toxic organic solvent, because they have good solubility and resolvability. However, with the development of biodiesel industry, the problem of raw material has become a major constraint to the further development of this industry. Because the cost of the oil-containing material takes more than 70% cost of the biodiesel product, a lot of researches focus on the cheap raw materials. In another aspect, China produces more than 10,000,000 tons of rice bran annually and most of the rice bran is utilized unreasonably. As realized the problems of these two areas, we used low quality rice bran to produce FAME and FAEE in this dissertation, which is killing two birds with one stone. Based on the research, we made integrated strategies of rice bran utilization, too.
Firstly, we need to design a process which could produce FAME and FAEE from low quality feedstock oil. Traditionally, the typical method using low quality oil to produce FAME and FAEE is two-step process. The first step is an acid catalyzed process, which esterifies free fatty acids (FFAs), and the second step is an alkaline catalyzed process, which transesterifies the glycerides in the feedstock. However, the intermediate treatment process between esterification and transesterificaion processes is a tedious procedure including neutralization of acid catalyst, removal of water and impurities, evaporation of alcohol or settlement for phase-separation, et al. The tedious work not only wastes a lot of time, but also produces waste water which is unfriendly to the environment. In our work, we evolved a simple route for the production of FAME and FAEE, by using the mixture of soybean oil and oleic acid (OA) as feedstock to imitate low quality lipids with substantial FFAs content. The merit of our route is that the intermediate process could be eliminated based on our designed experimental apparatus, thus acid and alkaline catalyzed processes performed without intervals. The water in the reaction system was eliminated simultaneously when it was formed by introduction of CaO powder to Soxhlet apparatus. On considering the environmental character of the whole strategy, the waste water and CaO residue were used as raw materials to produce value-added nano-CaCO3 byproduct via carbonation method at room temperature. Based on our strategy, the production process of FAME and FAEE could be simplified and the production cost could be reduced. It was an economical route for FAME and FAEE production.
Secondly, based on the designed process, we studied the production of FAEE from low quality rice bran. The effects of solvent, acid and alkaline catalysts on the yield rate, esterification rate and transesterification rate were studied. 12.29% ( w FAEE / wrice?bran) of FAEE was obtained when absolute ethanol was used as solvent to extract rice bran oil. The esterification rate and transesterification rate reached 97.90 % and 82.78 %, respectively. With the aid of petroleum ether, the yield rate of FAEE could be improved to 15.50% ( w FAEE / wrice?bran), and the esterification rate and transesterification rate reached 98.89% and 85.94%. Moreover, we found that the petroleum ether could restrain saponification in the case of FAEE production.
Thirdly, we further studied the production of FAME from low quality rice bran. The oil extraction process and the effect of petroleum ether on the esterification and transesterification processes were investigated. Besides, the moister resistance of the system was investigated, too. The results approved that the designed process was feasible. It was different from FAEE that we found there was a synergistic effect between methanol and petroleum ether. Less methanol and acid catalyst could be used because of this effect. When 50 g of rice bran, 75 mL of absolute methanol, 150 mL of petroleum ether, 0.75 g of concentrated sulfuric acid and 0.71 g of sodium hydroxyl were used, 16.69% ( w FAME / wrice?bran) of FAME was obtained. The esterification rate and the transesterification rate reached 98.83% and 80.47%.
Finaly, on considering the environmental character of the whole strategy, we investigated the utilization of the waste water and CaO residue from FAME and FAEE production. In this chapter, value-added calcium carbonate (CaCO3) with micro/nanostructures was produced via carbonation method at ambient temperature. The results showed that the CaCO3 obtained was hydrophobic (contact angle, 111o) and had broccoli-like morphology. It was made up of many uniform nano-rods, and each rod was composed of smaller particles with diameters about 50 nm. The idea of wastes utilization could make the FAME/FAEE production process environmentally friendly, and the income of the produced CaCO3 could further compensate the cost of FAME/FAEE production.
The integrated utilization of rice bran is a promising project. As a result, at the end of the dissertation, we designed some technical flows for the further investigation of rice bran and hope it would be useful for the coming works.
引文
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