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1、DOI:10.13982/j.mfst.1673-9078.2013.10.035现代食品科技ModernFoodScienceandTechnology2013,Vol.29,No.10白酒丢糟制备微晶纤维素工艺优化及结构特性1,212223任海伟,李金平,张轶,张飞,李志忠,向双全(1.兰州理工大学西部能源与环境研究中心,甘肃兰州730050)(2.兰州理工大学生命科学与工程学院,甘肃兰州730050)(3.甘肃金徽酒股份有限公司,甘肃陇南742308)摘要:白酒丢糟(DG)是一种富含纤维素的木质纤维素生物质,为充分转化利用丢糟资源,探
2、索其制备药用辅料微晶纤维素(MCC)的可行性。从丢糟中提取出高纯度纤维素,采用稀盐酸水解法制备丢糟微晶纤维素(DGMCC),考察了盐酸浓度、时间、温度和料液比等因素对产品聚合度和得率的影响,并通过正交实验优化制备工艺。结果表明,从丢糟中提取的纤维素纯度为94.55%;丢糟纤维素在料液比为1:15(g/mL)、盐酸浓度为6%(V/V)、温度为70℃的最优条件下水解60min可制得聚合度为288的DGMCC产品,得率为27.01%。利用FTIR、SEM、XRD、TGA和DSC等手段对DGMCC微观形貌、结晶结构和热稳定性进行表征。FTIR说明D
3、GMCC的主要成分为纤维素;SEM和XRD表明DGMCC呈不规则球形颗粒,纤维素晶型为Ⅰ型,相对结晶度为62.47%,晶粒尺寸为54.95nm。TGA和DSC表明DGMCC在365.3℃处有一尖锐的结晶熔融吸热峰,初始热分解温度高于原料DG,热稳定性好。关键词:白酒丢糟;微晶纤维素;聚合度;得率;结构特性文章篇号:1673-9078(2013)10-2461-2468OptimizationofPreparationConditionsandStructuralPropertiesofMicrocrystallineCellulosefro
4、mDistillersGrains1,212223RENHai-wei,LIJin-ping,ZHANGYi,ZHANGFei,LIZhi-zhong,XIANGShuang-quan(1.WesternChinaEnergy&EnvironmentResearchCenter,LanzhouUniversityofTechnology,Lanzhou730050,China)(2.SchoolofLifeScienceandEngineering,LanzhouUniversityofTechnology,Lanzhou730050,Ch
5、ina)(3.GansuJinhuiLiquorIndustryGroupGroupCO.,Ltd,Longnan742308,China)Abstract:Distillersgrain(DG)isakindoflignocellulosicbiomasswithhighcontentofcellulose.Inthisstudy,thefeasibilityofpreparingmicrocrystallinecellulose(MCC)byDGwasobserved.Dilutehydrochloricacidhydrolysiswa
6、scarriedouttoprepareDGMCC.ThepreparedDGMCCsampleswerethencharacterizedbyFTIR,SEM,XRD,TGAandDSC,comparingwiththatofDGandcommercialMCC®(LowaPH101).Thefinenessofcellulosewas94.55%.TheoptimumconditionsforthepreparationofDGMCCweresolid-liquidratioof1:15(g/mL),hydrochloricacidco
7、ncentrationsof6%(V/V),temperatureof70℃andtimeof60min,underwhichtheDPandtheyieldofDGMCCwere288and27.01%,respectively.FTIRspectroscopyshowedthatthemaincomponentofDGMCCwascellulose.SEMandXRDindicatedthattheDGMCCsamplesappearedanirregularbutoverallsphericalshape,thecrystallini
8、tyandparticlesizedofwhichwas62.47%and54.95nm,respectively.Inaddition,TGAandDSCrevealedash