Selective Isolation, Analysis And Esterification Of The Oil From Rice Husk Pyrolysis

Fuel and non-fuel employments are important two parts in biomass liquefied oil usage. However, there are few reports on non-fuel employment of biomass liquefied oil due to the complexion of it.In this paper, oil from rice husk liquefacation was separated by water under centrifugalization into two part, as water soluble part and water insoluble part, respectively. They were fatherly extracted with organic solvent, such as petroleum ether, carbon disulfide, chloroform, diethyl ether and acetic ether by step, the extract from which was analyzed by GC/MS. The result has shown the better solubility of rice husk liquefied oil in chloroform, diethyl ether and acetic ether, in which the extract ratio reaches more than 15%. It has shown us a complex component of rice husk liquefied oil, which mainly contains phenols, ketones, aldehydes, esters, acids and alkanes. Most compounds carry oxygen, such as hydroxyl and methoxyl. Carboxylic acids gift the oil acidity. Anthracene, humble and acylamino were also detected from these extracts. Different compounds exist in these two parts of rice husk liquefied oil, and those extracts by different solvents. Especially, alkanes from insoluble part are detected in benzene, which has reached as high as 57%. 4-hydroxyl, 3-methoxyl- benzaidehyde, a useful compound in rice husk liquefied oil, can be extracted with some solvents such as PE and carbon disulfide. It is detected that there are more non-aromatics in the product of aging rice husk liquefied oil that oxidized by sodium hypochlorite, which means the non-aromatics take important role in the aging reaction of the rice husk liquefied oil.The phase separating ability of different organic solvent / salt aqueous two-phase systems (ATPS), which testified that sodium dihydrogen phosphate / ethanol ATPS had good effects on phase separation and extraction to rice husk liquefied oil. The operating conditions of the ATPS was optimized, in which system the condition was 38.5% (w/w) sodium dihydrogen phosphate and 15.4% (w/w) ethanol, and was arranged to upgrade the rice husk liquefied oil. The rice husk liquefied oil in the upper layer of ATPS was upgraded by catalytic esterification, after which the average distillation of esterification oil, 60 oC-85 oC, 85 oC-95 oC and residue fraction were investigated. The distillation fractions were analyzed by GC/MS. The effects of the rice husk liquefied oil upgraded by aqueous two-phase extraction and esterification with the rice husk liquefied oil upgraded just by esterfication were compared. Column chromatography was arranged to extract the rice husk liquefied oil distillated after upgraded by ATPS, and the extraction fraction were analyzed by GC/MS. By measuring the distribution coefficient of main components in rice husk liquefied oil, the present author studied the distribution behavior of model compounds in ATPS. Experimental results show that:The water content of rice husk liquefied oil was upgraded by ATPS decreased by 34.8%. Catalytic esterification can raise the pH of these two esterification oils. The content of 60-85 oC fractions of esterification from the rice husk liquefied oil treated by ATPS and the crude rice husk liquefied oil are 63% and 67.7%, respectively. The detected compositions of the distillation fractions from these two upgraded esterification oil are similar, which contain hydrocarbons, phenolic compounds, ketones and aldehydes. Meanwhile, it is found that esters in which was treated ATPS were far more than those in rice husk liquefied oil, after esterification. Through the separation and analysis of phase from the rice husk liquefied oil upgraded by ATPS, the study shows that ATPS can be used to extract L-glucan from rice husk liquefied oil. The study of the distribution behavior of ATPS model compounds can provide a theoretical basis for the distribution behavior of rice husk liquefied oil extraction in ATPS.The mechanism of the reaction between rice husk liquefied oil and ammonia was studied. It is discovered that 3,5-dimethyl-2-oxazoline-4-methanol can be obtained by the reaction between pure hydroxyl acetone and ammonia, while with acetic acid in acidic condition, pyridines and pyrazines are obtained. The optimized temperature, time and the concentration of ammonia for the reaction between hydroxyl acetone and ammonia in micro wave are 90oC, 10min and 15%, respectively.