高酸值花椒籽油酯化脱酸的工艺研究
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摘要
本研究以花椒籽油为基本原料,花椒籽油一般颜色较深、酸价较高,本文有针对性的先对花椒籽油进行脱色,再以酯化脱酸的方法对花椒籽油进行精炼,最后对酯化油进行必要的后处理,精炼效果较好。
在脱色工艺的研究中,以活性炭结合活性白土作为混合脱色剂,重点研究活性炭占混合脱色剂比例、混合脱色剂用量、脱色时间、脱色温度四个脱色影响因素,结合单因素试验和响应面优化试验,最终得出最佳的脱色条件为∶活性炭占混合脱色剂比例∶15.5%;混合脱色剂用量∶2%;脱色时间∶22min;脱色温度∶93℃,在此条件下脱色率为79.71%。
在酯化脱酸工艺研究中,对五种传统的酯化催化剂进行比较筛选,结果表明ZnO催化效果最好。选定ZnO作为酯化反应的催化剂,对酯化反应时间、酯化反应温度、ZnO添加量、单甘酯/甘油(1∶1,w/w)添加量进行单因素试验考察,并进行正交试验分析。通过正交试验分析并结合单因素试验情况,综合考虑酯化温度对酯化油色泽的影响和经济适用性,最终确定最佳的酯化条件为∶酯化时间6h、酯化温度200℃、ZnO添加量为0.2%、单甘酯/甘油(1∶1,w/w)添加量为理论添加量的150%,在此条件下得到的酯化油的酸价为3.57mgKOH/g,酯化油中单甘酯、甘二酯的含量分别为3.25%、13.64%。
酯化油的后处理主要是对甘油三酯进行纯化,纯化采用溶剂萃取法,萃取条件为∶萃取剂采用乙醇,浓度为85%;乙醇溶液/混合油(w/w)比例为0.8∶1;萃取温度为40℃,最终得到的甘油三酯中单甘酯含量为0.88%,甘二酯含量为4.62%,酸价降至1.73 mgKOH/g。
In this study, the basic raw material was prickly ash seed oil, prickly ash seed oil was generally dark in color, and had higher acid value, the text targeted for decolorizing the prickly ash seed oil pertinencily, then refining oil by the way of acid esterification, finally depickling with esterificating the oil post-processing necessarily, that refined results were better.
In the study of discolor process, activated carbon combined with activated clay as a mixed-decolorizing agent, focused on four decolorizing factors,including of activated carbon accounting for the mixed-decolorizing agent , mixed-decolorizing agent dosage,decolorizing time, and decolorizing temperature. Combining single factor experiment and response surface optimization experiments , ultimately optimum decolorizing conditions were as follow∶activated carbon accounting for the mixed- decolorizing agent 15.5% ; mixed-decolorizing dosage 2% ; decolorizing time 22min ; decolorizing temperature 93℃, under the optimum conditions,the decolorizing rate was 79.71%.
In the study of depickling with esterification process , by comparing five traditional esterification catalyst screening,the results showed that the catalyst ZnO was the best. Selected ZnO as a catalyst for esterification, we used the reaction time on esterification, esterification temperature, the dosage of ZnO, the addition of monoglyceride / glycerine (1∶1,w/w) as the single factor experiment for observation and analysis of orthogonal test. Through orthogonal test analysis of single factor experiments combined with the situation, considering the effect on oil color by reaction temperature on the esterification and economic applicability,finally determined the optimal reaction conditions were as follows∶reaction temperature 200℃, the dosage of ZnO 0.2%,monoglyceride / glycerine (1∶1,w/w) content 150% of the theoretical value, under this condition, the acid ester oil price was 3.57mgKOH / g, the yield of monoglyceride and diglyceride in the ester oil were 3.25% and 13.64% respectively.
In the post-processing of oil esterification,mainly purified triglyceride by solvent extraction, extraction conditions were as follow∶extraction solvent 85% ethanol concentration; ethanol / mixed oil (w/w) percentage was0.8∶1; extraction temperature 40℃, finally the content of triglycerides in monoglyceride was 0.88%, the content of diglyceride was 4.62%, acid value dropped to 1.73 mgKOH / g.
在脱色工艺的研究中,以活性炭结合活性白土作为混合脱色剂,重点研究活性炭占混合脱色剂比例、混合脱色剂用量、脱色时间、脱色温度四个脱色影响因素,结合单因素试验和响应面优化试验,最终得出最佳的脱色条件为∶活性炭占混合脱色剂比例∶15.5%;混合脱色剂用量∶2%;脱色时间∶22min;脱色温度∶93℃,在此条件下脱色率为79.71%。
在酯化脱酸工艺研究中,对五种传统的酯化催化剂进行比较筛选,结果表明ZnO催化效果最好。选定ZnO作为酯化反应的催化剂,对酯化反应时间、酯化反应温度、ZnO添加量、单甘酯/甘油(1∶1,w/w)添加量进行单因素试验考察,并进行正交试验分析。通过正交试验分析并结合单因素试验情况,综合考虑酯化温度对酯化油色泽的影响和经济适用性,最终确定最佳的酯化条件为∶酯化时间6h、酯化温度200℃、ZnO添加量为0.2%、单甘酯/甘油(1∶1,w/w)添加量为理论添加量的150%,在此条件下得到的酯化油的酸价为3.57mgKOH/g,酯化油中单甘酯、甘二酯的含量分别为3.25%、13.64%。
酯化油的后处理主要是对甘油三酯进行纯化,纯化采用溶剂萃取法,萃取条件为∶萃取剂采用乙醇,浓度为85%;乙醇溶液/混合油(w/w)比例为0.8∶1;萃取温度为40℃,最终得到的甘油三酯中单甘酯含量为0.88%,甘二酯含量为4.62%,酸价降至1.73 mgKOH/g。
In this study, the basic raw material was prickly ash seed oil, prickly ash seed oil was generally dark in color, and had higher acid value, the text targeted for decolorizing the prickly ash seed oil pertinencily, then refining oil by the way of acid esterification, finally depickling with esterificating the oil post-processing necessarily, that refined results were better.
In the study of discolor process, activated carbon combined with activated clay as a mixed-decolorizing agent, focused on four decolorizing factors,including of activated carbon accounting for the mixed-decolorizing agent , mixed-decolorizing agent dosage,decolorizing time, and decolorizing temperature. Combining single factor experiment and response surface optimization experiments , ultimately optimum decolorizing conditions were as follow∶activated carbon accounting for the mixed- decolorizing agent 15.5% ; mixed-decolorizing dosage 2% ; decolorizing time 22min ; decolorizing temperature 93℃, under the optimum conditions,the decolorizing rate was 79.71%.
In the study of depickling with esterification process , by comparing five traditional esterification catalyst screening,the results showed that the catalyst ZnO was the best. Selected ZnO as a catalyst for esterification, we used the reaction time on esterification, esterification temperature, the dosage of ZnO, the addition of monoglyceride / glycerine (1∶1,w/w) as the single factor experiment for observation and analysis of orthogonal test. Through orthogonal test analysis of single factor experiments combined with the situation, considering the effect on oil color by reaction temperature on the esterification and economic applicability,finally determined the optimal reaction conditions were as follows∶reaction temperature 200℃, the dosage of ZnO 0.2%,monoglyceride / glycerine (1∶1,w/w) content 150% of the theoretical value, under this condition, the acid ester oil price was 3.57mgKOH / g, the yield of monoglyceride and diglyceride in the ester oil were 3.25% and 13.64% respectively.
In the post-processing of oil esterification,mainly purified triglyceride by solvent extraction, extraction conditions were as follow∶extraction solvent 85% ethanol concentration; ethanol / mixed oil (w/w) percentage was0.8∶1; extraction temperature 40℃, finally the content of triglycerides in monoglyceride was 0.88%, the content of diglyceride was 4.62%, acid value dropped to 1.73 mgKOH / g.
引文
[1]张氽,阚建全,陈宗道.花椒籽的开发利用[J].中国调味品.2003(10)∶3-5.
[2]王志勇,邹洪.花椒籽的开发应用[J].北京教育学院学报.2007∶2(3)∶15-18.
[3]张庆勇.山西榆次花椒油的成分分析[J].香料香精化妆品,1996,(2)∶11-13.
[4]张庆勇.两种四川花椒油的成分分析[J].香料香精化妆品,1996,(3)∶20-22.
[5] Yoon H K,Kim,J M.Analytical studies on the composition of oil and protein in the seed of thornless chinese peper Zanthoxylum schinifolium var.inermis nakai[R].Reports of Agricultural Research and Technology Chungnam University (Korea Republic).1976,3(2)∶170-176.
[6] Ahmad F,Ahmad I,Osman S M.The C16 monoenoic acid of Zanthoxylum alatum seed oil[J].Journal of the American Oil Chemistsˊ Society(USA).1980,57(7)∶224-225.
[7] Venkatachalam S R , Hassrajani S A , Rane S S , Mamdapur V R. Cis-10-Octadecenoic acid,component of Zanthoxylum alatum seed oil[J].Indian journal of Chemistry Section B , Organic including Medicinal ( United Kingdom).1996,35(5)∶514-517.
[8]李桂华,付黎敏,薛开发.花椒种籽化学成分分析研究[J].郑州粮食学院学报,1994,15(4)∶17-l9.
[9]庄世宏,李盂楼.花椒籽油的成分分析.西北农业学报,2002,11(2)∶43-45.
[10]樊经建.花椒,花椒叶芳香油及花椒油的成分分析[J].中国油脂,1992(1)∶32-34.
[11]马传国等.花椒籽皮油和仁油化学成分分析[J].郑州工业学院学报,2003,23(1).
[12]唐宝奎.花椒籽-种亟待开发利用的油脂资源[J].中国野生植物,l992(2)∶24 -26.
[13]侯党社,陈栓虎.花椒籽油的酯化脱酸研究[J].宝鸡文理学院学报,2003,3(1)∶35-36.
[14]朱健,冯敏杰.花椒[M].西安∶陕西科学技术出版社,1993.
[15]李孟楼,郭新荣,谢恩魁等.花椒种子油的含蜡量测定与脱蜡[J].西北植物学报,2001,21(2)∶387-390.
[16]薛开发.花椒籽制油工艺技术[J].中国油脂,1999.24(4)∶12-13.
[17]苏望懿.米糠油的酯化脱酸[J].中国油酯,1992,17(增刊)∶122-126.
[18] ZHAO Jing.Method for extraction of edible spicy oils from spices[P].CN 1053259.CA116∶127353.
[19]刘军海,王勇.浅析影响油脂吸附脱色效果的因素[J].西部粮油科技.1998,23∶24-26.
[20]孙志芳,高荫榆,洪雪娥.植物油脱色研究进展[J].食品科技.2005(1)∶31-32.
[21]曹艳君.王好平.植物油的脱色研究[J].沈阳化工. 1998,1(27)∶15-17.
[22]朱振海,郑茂松.凹凸脱色剂对植物油脱色率及化学组份作用的探讨[J]非金属矿.1998.
[23]王丽娟.紫苏油脱色工艺条件的研究[J].粮油加工与机械.2004,7∶40-41.
[24]庞文胜,毛洗荣.茶油精制工艺初探[J].林业科技开发.2004,1(18)∶54-55
[25] Salm Omar,Badei Girgis.Carbonaceous materials from seed hulls for bleaching of vegetable oils[J].food research international. 2003,36∶11-17.
[26]李癑,陈正行.稻壳灰制取大豆精炼油中脱色剂的研究[J].中国油脂.2004,3(29)∶30-32.
[27]齐玉堂.深色油脂脱色工艺研究[J].粮食与油脂。2004,7∶28-29.
[28]梁少华,马传国.米糠深加工技术的分析与评价[J].中国油脂,2005,30(11)∶10-15.
[29]刘军海.米糠油精炼新技术.食品科技,2000,5∶4-5.
[30]刘军海,任慧兰.食用油脱酸新方法研究进展[J].粮食与油脂,2008,2∶1-6.
[31] Turkay S,Burford M D,et a1.Deacidifieation of black cumin seed oil by selective supercritical carbon dioxide extraction[J].Journal of the American oil Chemists’Society,1996,73∶1265-1270.
[32] Brunetti L , et a1.Deacidification of olive oils by supercritical carbon dioxide[J].Journal of the American oil Chemists’Society,1989,66∶209-217
[33] Ooi C K,Bhaskar A,et a1.Continuous supercritieal carbon dioxide processing of palm oil[J].Journal of the American oil Chemists’Society,1996,73∶233-237
[34] Ziegler G R,Liaw Y J.Deodorization and deacidification of edible oils with dense carbon dioxide[J].Journal of the American oil Chemists’Society,1993,70∶947-953.
[35]李桂华,徐广超,朱书爱.高酸价米糠油酯化脱酸的研究[J].郑州工程学院学报,2002,23(1)∶36-38.
[36]董建林,魏冰.高酸值油脂助脱色与酯化脱酸工艺的研究[J].中国油脂,2000,25(6)∶82-85.
[37]Millwalla R H , Shitole A D.Refining of the rice bran oil employingreesterification technique[J].Journal of the Oil Technologists’Association of India,1987,19∶70-71.
[38]Bhattacharyya A C,Bhattacharrya D K.Deacification of high FFA rice bran oil by reesterification and alkali neutralization[J].Journal of the American Oil Chemists’Society,1987,64∶128-131.
[39]Anand R,Vasishtha A K.Reesterification of rice bran oil of high free fatty acidity[J].Journal of the Oil Techonologists’Association of India,1978,10∶141-143.
[40] Bhattacharyya S, Bhattacharyya D K.Biorefining of high acid rice bran oil using a microorganism [J].Journal of the American Oil Chemists’Society,1989,66∶1469-1471.
[41] Sengupta R, Bhattacharyya D K.Effect of monoglycerides on enzymatic deacidification of rice bran oil [J].Journal of the Oil Technologists’Association of india,1996,28∶125-130.
[42]翟丹丹,张建法,蒋鹏举等.甘油二酯的制备、纯化及分析[J].河南化工2004,5∶4-6.
[43] Sugiura M, Yamada T. Production of diglyeerides and reactor for the production process[P].JP∶042165,1998-09-08.
[44] Holmherg K,Lassen B,Stark M B.Enzymatie glyeerolysis of a triglyceride in aqueous and nonaqueous micromulsions[J].J.Am.Oil Chem.Soe.,1989,66(12)∶1796-1800.
[45]孙登文,湛日景.用溶剂结晶法分离单脂肪酸甘油酯的工艺[P].ZL∶92100594.6,1992-01-31.
[46] Nguyen A.D.et al.Chem.Eng.Sci.1997,52(16)∶2661-2666.
[47] Holly C Pinkart,Richard Devereax,Peter J Chapman.Rapid separation of microbial lipids using solid phase extraction columns[J].Journal of Microbiological Methods,1998,34∶9-15.
[48]章朝晖,冯巧嫦.高纯度单脂肪酸甘油酯的制备[J].精细石油化工,2001,3(2)∶18-22.
[49] REVERCHON E,DELLA P G, GORGOGLIONE D. Supercritical CO2 fractionation of jasmine concrete[J]. J Supercritical Fluids, 1995(8)∶60-65.
[50]吴丽萍,李宏宇,陈雪峰.亚麻籽油脱色工艺的研究[J].资源开发与市场,2009,25(12)∶1057-1059
[51] GB 5525-1985,植物油脂检验透明度、色泽、气味、滋味鉴定法[S].
[52]孙凤霞,杜红霞,周展明.油脂色泽测定方法研究进展[J].四川粮油科技,2002,4(76)∶54-56.
[53]齐志国,史高峰,韩舜愈等.活性凹凸棒土对大麻籽油脱色的研究[J].中国油脂,2007,32(8)∶67-69.
[54] Sayer.R.N,Nayyar.D.K,Sauders.M.Extraction and refining of edible oil from extrusion stabilized rice bran[J].JACICS,1985,62(6)∶1040-1043.
[55]苏望懿.油脂加工工艺学[M].武汉∶湖北科学技术出版社,1998.
[56]刘玉兰.油脂制取与加工工艺学[M].科学出版社,2003.
[57] Earopean Journal of Lipid Science and Technology,2001,103(7)∶505-515.
[58] Y.H.Hui.贝雷∶油脂化学与工艺学[M].中国轻工业出版社,2001.
[59]朱屯,李洲等.溶剂萃取[M].化学工业出版社,2008.
[60]刘晔.高酸值米糠油萃取脱酸工艺的研究[J].粮油加工,2005,12∶48-52.
[61]孙登文,湛日景.用溶剂结晶法分离单脂肪酸甘油酯的工艺[p].ZL∶92100594.6,1992-01-31.
[2]王志勇,邹洪.花椒籽的开发应用[J].北京教育学院学报.2007∶2(3)∶15-18.
[3]张庆勇.山西榆次花椒油的成分分析[J].香料香精化妆品,1996,(2)∶11-13.
[4]张庆勇.两种四川花椒油的成分分析[J].香料香精化妆品,1996,(3)∶20-22.
[5] Yoon H K,Kim,J M.Analytical studies on the composition of oil and protein in the seed of thornless chinese peper Zanthoxylum schinifolium var.inermis nakai[R].Reports of Agricultural Research and Technology Chungnam University (Korea Republic).1976,3(2)∶170-176.
[6] Ahmad F,Ahmad I,Osman S M.The C16 monoenoic acid of Zanthoxylum alatum seed oil[J].Journal of the American Oil Chemistsˊ Society(USA).1980,57(7)∶224-225.
[7] Venkatachalam S R , Hassrajani S A , Rane S S , Mamdapur V R. Cis-10-Octadecenoic acid,component of Zanthoxylum alatum seed oil[J].Indian journal of Chemistry Section B , Organic including Medicinal ( United Kingdom).1996,35(5)∶514-517.
[8]李桂华,付黎敏,薛开发.花椒种籽化学成分分析研究[J].郑州粮食学院学报,1994,15(4)∶17-l9.
[9]庄世宏,李盂楼.花椒籽油的成分分析.西北农业学报,2002,11(2)∶43-45.
[10]樊经建.花椒,花椒叶芳香油及花椒油的成分分析[J].中国油脂,1992(1)∶32-34.
[11]马传国等.花椒籽皮油和仁油化学成分分析[J].郑州工业学院学报,2003,23(1).
[12]唐宝奎.花椒籽-种亟待开发利用的油脂资源[J].中国野生植物,l992(2)∶24 -26.
[13]侯党社,陈栓虎.花椒籽油的酯化脱酸研究[J].宝鸡文理学院学报,2003,3(1)∶35-36.
[14]朱健,冯敏杰.花椒[M].西安∶陕西科学技术出版社,1993.
[15]李孟楼,郭新荣,谢恩魁等.花椒种子油的含蜡量测定与脱蜡[J].西北植物学报,2001,21(2)∶387-390.
[16]薛开发.花椒籽制油工艺技术[J].中国油脂,1999.24(4)∶12-13.
[17]苏望懿.米糠油的酯化脱酸[J].中国油酯,1992,17(增刊)∶122-126.
[18] ZHAO Jing.Method for extraction of edible spicy oils from spices[P].CN 1053259.CA116∶127353.
[19]刘军海,王勇.浅析影响油脂吸附脱色效果的因素[J].西部粮油科技.1998,23∶24-26.
[20]孙志芳,高荫榆,洪雪娥.植物油脱色研究进展[J].食品科技.2005(1)∶31-32.
[21]曹艳君.王好平.植物油的脱色研究[J].沈阳化工. 1998,1(27)∶15-17.
[22]朱振海,郑茂松.凹凸脱色剂对植物油脱色率及化学组份作用的探讨[J]非金属矿.1998.
[23]王丽娟.紫苏油脱色工艺条件的研究[J].粮油加工与机械.2004,7∶40-41.
[24]庞文胜,毛洗荣.茶油精制工艺初探[J].林业科技开发.2004,1(18)∶54-55
[25] Salm Omar,Badei Girgis.Carbonaceous materials from seed hulls for bleaching of vegetable oils[J].food research international. 2003,36∶11-17.
[26]李癑,陈正行.稻壳灰制取大豆精炼油中脱色剂的研究[J].中国油脂.2004,3(29)∶30-32.
[27]齐玉堂.深色油脂脱色工艺研究[J].粮食与油脂。2004,7∶28-29.
[28]梁少华,马传国.米糠深加工技术的分析与评价[J].中国油脂,2005,30(11)∶10-15.
[29]刘军海.米糠油精炼新技术.食品科技,2000,5∶4-5.
[30]刘军海,任慧兰.食用油脱酸新方法研究进展[J].粮食与油脂,2008,2∶1-6.
[31] Turkay S,Burford M D,et a1.Deacidifieation of black cumin seed oil by selective supercritical carbon dioxide extraction[J].Journal of the American oil Chemists’Society,1996,73∶1265-1270.
[32] Brunetti L , et a1.Deacidification of olive oils by supercritical carbon dioxide[J].Journal of the American oil Chemists’Society,1989,66∶209-217
[33] Ooi C K,Bhaskar A,et a1.Continuous supercritieal carbon dioxide processing of palm oil[J].Journal of the American oil Chemists’Society,1996,73∶233-237
[34] Ziegler G R,Liaw Y J.Deodorization and deacidification of edible oils with dense carbon dioxide[J].Journal of the American oil Chemists’Society,1993,70∶947-953.
[35]李桂华,徐广超,朱书爱.高酸价米糠油酯化脱酸的研究[J].郑州工程学院学报,2002,23(1)∶36-38.
[36]董建林,魏冰.高酸值油脂助脱色与酯化脱酸工艺的研究[J].中国油脂,2000,25(6)∶82-85.
[37]Millwalla R H , Shitole A D.Refining of the rice bran oil employingreesterification technique[J].Journal of the Oil Technologists’Association of India,1987,19∶70-71.
[38]Bhattacharyya A C,Bhattacharrya D K.Deacification of high FFA rice bran oil by reesterification and alkali neutralization[J].Journal of the American Oil Chemists’Society,1987,64∶128-131.
[39]Anand R,Vasishtha A K.Reesterification of rice bran oil of high free fatty acidity[J].Journal of the Oil Techonologists’Association of India,1978,10∶141-143.
[40] Bhattacharyya S, Bhattacharyya D K.Biorefining of high acid rice bran oil using a microorganism [J].Journal of the American Oil Chemists’Society,1989,66∶1469-1471.
[41] Sengupta R, Bhattacharyya D K.Effect of monoglycerides on enzymatic deacidification of rice bran oil [J].Journal of the Oil Technologists’Association of india,1996,28∶125-130.
[42]翟丹丹,张建法,蒋鹏举等.甘油二酯的制备、纯化及分析[J].河南化工2004,5∶4-6.
[43] Sugiura M, Yamada T. Production of diglyeerides and reactor for the production process[P].JP∶042165,1998-09-08.
[44] Holmherg K,Lassen B,Stark M B.Enzymatie glyeerolysis of a triglyceride in aqueous and nonaqueous micromulsions[J].J.Am.Oil Chem.Soe.,1989,66(12)∶1796-1800.
[45]孙登文,湛日景.用溶剂结晶法分离单脂肪酸甘油酯的工艺[P].ZL∶92100594.6,1992-01-31.
[46] Nguyen A.D.et al.Chem.Eng.Sci.1997,52(16)∶2661-2666.
[47] Holly C Pinkart,Richard Devereax,Peter J Chapman.Rapid separation of microbial lipids using solid phase extraction columns[J].Journal of Microbiological Methods,1998,34∶9-15.
[48]章朝晖,冯巧嫦.高纯度单脂肪酸甘油酯的制备[J].精细石油化工,2001,3(2)∶18-22.
[49] REVERCHON E,DELLA P G, GORGOGLIONE D. Supercritical CO2 fractionation of jasmine concrete[J]. J Supercritical Fluids, 1995(8)∶60-65.
[50]吴丽萍,李宏宇,陈雪峰.亚麻籽油脱色工艺的研究[J].资源开发与市场,2009,25(12)∶1057-1059
[51] GB 5525-1985,植物油脂检验透明度、色泽、气味、滋味鉴定法[S].
[52]孙凤霞,杜红霞,周展明.油脂色泽测定方法研究进展[J].四川粮油科技,2002,4(76)∶54-56.
[53]齐志国,史高峰,韩舜愈等.活性凹凸棒土对大麻籽油脱色的研究[J].中国油脂,2007,32(8)∶67-69.
[54] Sayer.R.N,Nayyar.D.K,Sauders.M.Extraction and refining of edible oil from extrusion stabilized rice bran[J].JACICS,1985,62(6)∶1040-1043.
[55]苏望懿.油脂加工工艺学[M].武汉∶湖北科学技术出版社,1998.
[56]刘玉兰.油脂制取与加工工艺学[M].科学出版社,2003.
[57] Earopean Journal of Lipid Science and Technology,2001,103(7)∶505-515.
[58] Y.H.Hui.贝雷∶油脂化学与工艺学[M].中国轻工业出版社,2001.
[59]朱屯,李洲等.溶剂萃取[M].化学工业出版社,2008.
[60]刘晔.高酸值米糠油萃取脱酸工艺的研究[J].粮油加工,2005,12∶48-52.
[61]孙登文,湛日景.用溶剂结晶法分离单脂肪酸甘油酯的工艺[p].ZL∶92100594.6,1992-01-31.