Microwave freeze-drying of vitamin C solution frozen with preformed pores

ZHANG Shuo; WANG Wei; LI Qiangqiang; TANG Yujia; DONG Tieyou

doi:10.11949/j.issn.0438-1157.20181487

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Microwave freeze-drying of vitamin C solution frozen with preformed pores

Fluid dynamics and transport phenomena | 更新时间：2026-07-24

- Microwave freeze-drying of vitamin C solution frozen with preformed pores
- CIESC Journal Vol. 70, Issue 6, Pages: 2129-2138(2019)
- 作者机构：
  
  1.大连理工大学化工机械与安全学院，辽宁大连 116024
  2.河南科技大学农业装备工程学院，河南洛阳 471003
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20181487
  CLC： TQ 028.5;TQ 026.6;TQ 025.1
- Received：17 December 2018，
  
  Revised：2019-03-18，
  
  Online First：15 June 2020，
  
  Published：05 June 2019
- 稿件说明：
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张朔, 王维, 李强强, 唐宇佳, 董铁有. 具有预制孔隙的维生素C水溶液微波冷冻干燥[J]. 化工学报, 2019, 70(6): 2129-2138

ZHANG Shuo, WANG Wei, LI Qiangqiang, TANG Yujia, DONG Tieyou. Microwave freeze-drying of vitamin C solution frozen with preformed pores[J]. CIESC Journal, 2019, 70(6): 2129-2138
张朔, 王维, 李强强, 唐宇佳, 董铁有. 具有预制孔隙的维生素C水溶液微波冷冻干燥[J]. 化工学报, 2019, 70(6): 2129-2138 DOI： 10.11949/j.issn.0438-1157.20181487.

ZHANG Shuo, WANG Wei, LI Qiangqiang, TANG Yujia, DONG Tieyou. Microwave freeze-drying of vitamin C solution frozen with preformed pores[J]. CIESC Journal, 2019, 70(6): 2129-2138 DOI： 10.11949/j.issn.0438-1157.20181487.

摘要

设计和组装了一套实验室规模的多功能微波冷冻干燥装置，探究了具有初始孔隙的非饱和物料微波冷冻干燥过程。以维生素C为溶质，采用“软冰”冷冻技术制备了初始饱和与非饱和的冷冻样品。结果表明，软冰冷冻制备的样品能够避免崩塌。在35℃和20 Pa条件下，初始非饱和物料的干燥时间比饱和物料缩短了30.4%。SEM表征显示，非饱和物料具有疏松的球状孔隙结构、连通性好，有利于水蒸气的迁移。采用吸波材料碳化硅辅助的微波加热能够进一步强化冷冻干燥过程。在相同条件下，非饱和物料的微波冷冻干燥(5 W功率)时间比常规冷冻干燥(0 W功率)缩短了28.1%，比饱和物料的常规冷冻干燥缩短了50.0%。吸波材料辅助的初始非饱和物料微波冷冻干燥实现了传热传质的同时强化。

Abstract

A lab-scale multifunctional microwave freeze-dryer was designed and assembled to explore the microwave freeze-drying process of initially unsaturated frozen material with preformed pores. Initially saturated and unsaturated frozen samples were prepared by using“soft ice”freezing technique using vitamin C as the solute. The results showed that the saturated sample by soft ice freezing can effectively avoid structural collapse during freeze-drying

and the initially unsaturated frozen material can significantly enhance the freeze-drying process. Under 35℃ of the ambient radiation temperature and 20 Pa of the drying chamber pressure

the initially unsaturated sample saved 30.4% of drying time compared with the saturated one. SEM images of dried products revealed that the initial unsaturated material had a loose solid substrate and a spherical pore structure

which is favorable to the migration of sublimated/desorbed vapor. Appropriate increasing the radiation temperature was conducive to reducing the drying time and changing the chamber pressure had insignificant effect on freeze-drying. With a wave-absorbing material―silicon carbide (SiC) as the supporting pad of sample

microwave heating can further enhance the freeze-drying process. Under the same operating conditions

the drying time for microwave freeze-drying (5 W input) of the unsaturated sample can be 28.1% shorter than that for conventional freeze-drying (0 W input)

and 50.0% shorter than that for conventional freeze-drying of the saturated sample. SiC assisted microwave freeze-drying of the initially unsaturated frozen material is a feasible way to achieve the simultaneous enhancement of heat and mass transfer in freeze-drying.

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references

Padayatty S J , Katz A , Wang Y , et al . Vitamin C as an antioxidant: evaluation of its role in disease prevention [J ] . Journal of the American College of Nutrition , 2003 , 22 ( 1 ): 18 - 35 .

Medicine I O ， Vitamin C . Dietary Reference Intakes for Vitamin C, Vitamin E, Selenium, and Carotenoids [M ] . Washington : National Academies Press , 2000 : 95 - 185 .

刘艳玲 , 王英 , 胥清泉 , 等 . 一种注射用维生素C冻干粉针及其制备方法 : 103239414A [P ] . 2013-08-14 .

Liu Y L , Wang Y , Xu Q Q , et al . A kind of freeze-dried vitamin C powder for injection and its preparation process : 103239414A [P ] . 2013-08-14 .

Wang W , Chen G H . Physical interpretation of solid drying: an overview on mathematical modeling research [J ] . Drying Technology , 2007 , 25 ( 4 ): 659 - 668 .

Ratti C . Hot air and freeze-drying of high-value foods: a review [J ] . Journal of Food Engineering , 2001 , 49 ( 4 ): 311 - 319 .

Pikal M J . Freeze drying [M ] // Swarbrick J. Encyclopedia of Pharmaceutical Technology . New York : Informa Healthcare , 2007 : 1807 - 1833 .

Liapis A I , Bruttini R . Freeze drying [M ] // Mujumdar A S. Handbook of Industrial Drying . New York : CRC Press , 2015 : 259 - 282 .

Wang W , Chen G H . Numerical investigation on dielectric material assisted microwave freeze-drying of aqueous mannitol solution [J ] . Drying Technology , 2003 , 21 ( 6 ): 995 - 1017 .

Wang W , Chen G H . Heat and mass transfer model of dielectric-material-assisted microwave freeze-drying of skim milk with hygroscopic effect [J ] . Chemical Engineering Science , 2005 , 60 ( 23 ): 6542 - 6550 .

Wang W , Chen G H . Freeze drying with dielectric-material-assisted microwave heating [J ] . AIChE Journal , 2007 , 53 ( 12 ): 3077 - 3088 .

Capozzi L C , Pisano R . Looking inside the ‘black box : freezing engineering to ensure the quality of freeze-dried biopharmaceuticals [J ] . European Journal of Pharmaceutics and Biopharmaceutics , 2018 , 129 ( 8 ): 58 - 65 .

Goshima H , Do G , Nakagawa K . Impact of ice morphology on design space of pharmaceutical freeze-drying [J ] . Journal of Pharmaceutical Sciences , 2016 , 105 ( 6 ): 1920 - 1933 .

Millman M J , Liapis A I , Marchello J M . An analysis of the lyophilization process using a sorption-sublimation model and various operational policies [J ] . AIChE Journal , 1985 , 31 ( 10 ): 1594 - 1604 .

Petropoulos J H , Petrou J K , Liapis A I . Network model investigation of gas transport in bidisperse porous adsorbents [J ] . Industrial & Engineering Chemistry Research , 1991 , 30 ( 6 ): 1281 - 1289 .

Saclier M , Peczalski R , Andrieu J . Effect of ultrasonically induced nucleation on ice crystals size and shape during freezing in vials [J ] . Chemical Engineering Science , 2010 , 65 ( 10 ): 3064 - 3071 .

Sitar A , Skrlec K , Voglar J , et al . Effects of controlled nucleation on freeze-drying lactose and mannitol aqueous solutions [J ] . Drying Technology , 2018 , 36 ( 10 ): 1263 - 1272 .

Searles J A , Carpenter J F , Randolph T W . Annealing to optimize the primary drying rate, reduce freezing-induced drying rate heterogeneity, and determine T ' g in pharmaceutical lyophilization [J ] . Journal of Pharmaceutical Sciences , 2001 , 90 ( 7 ): 872 - 887 .

Bexiga N M , Bloise A C , Alencar A M , et al . Freeze-drying of ovalbumin-loaded carboxymethyl chitosan nanocapsules: impact of freezing and annealing procedures on physicochemical properties of the formulation during dried storage [J ] . Drying Technology , 2018 , 36 ( 4 ): 400 - 417 .

Oddone I , Pisano R , Bullich R , et al . Vacuum-induced nucleation as a method for freeze-drying cycle optimization [J ] . Industrial & Engineering Chemistry Research , 2014 , 53 ( 47 ): 18236 - 18244 .

Oddone I , Barresi A A , Pisano R . Influence of controlled ice nucleation on the freeze-drying of pharmaceutical products: the secondary drying step [J ] . International Journal of Pharmaceutics , 2017 , 524 ( 1/2 ): 134 - 140 .

于凯 , 王维 , 潘艳秋 , 等 . 初始非饱和多孔物料对冷冻干燥过程的影响 [J ] . 化工学报 , 2013 , 64 ( 9 ): 3110 - 3116 .

Yu K , Wang W , Pan Y Q , et al . Effect of initially unsaturated porous frozen material on freeze-drying [J ] . CIESC Journal , 2013 , 64 ( 9 ): 3110 - 3116 .

Wang W , Hu D P , Pan Y Q , et al . Freeze-drying of aqueous solution frozen with prebuilt pores [J ] . AIChE Journal , 2015 , 61 ( 6 ): 2048 - 2057 .

牛利娇 , 王维 , 潘思麒 , 等 . 具有预制孔隙多孔介质冷冻干燥的多相传递模型 [J ] . 化工学报 , 2017 , 68 ( 5 ): 1833 - 1844 .

Niu L J , Wang W , Pan S Q , et al . Multiphase transport model for freeze-drying of porous media with prefabricated porosity [J ] . CIESC Journal , 2017 , 68 ( 5 ): 1833 - 1844 .

李恒乐 , 王维 , 李强强 , 等 . 具有预制孔隙多孔物料的冷冻干燥 [J ] . 化工学报 , 2016 , 67 ( 7 ): 2857 - 2863 .

Li H L , Wang W , Li Q Q , et al . Freeze-drying of porous frozen material with prefabricated porosity [J ] . CIESC Journal , 2016 , 67 ( 7 ): 2857 - 2863 .

Wang W , Hu D P , Pan Y Q , et al . Numerical investigation on freeze-drying of aqueous material frozen with pre-built pores [J ] . Chinese Journal of Chemical Engineering , 2016 , 24 ( 1 ): 116 - 125 .

Chen G , Wang W , Mujumdar A S . Theoretical study of microwave heating patterns on batch fluidized bed drying of porous material [J ] . Chemical Engineering Science , 2001 , 56 ( 24 ): 6823 - 6835 .

Bahl I J , Bhartia P . Microwave Solid State Circuit Design [M ] . New York : John Wiley & Sons Inc ., 2003 : 1 - 15 .

远坂俊昭 . 锁相环(PLL)电路设计与应用 [M ] . 何希才, 译. 北京 : 科学出版社 , 2006 : 31 - 51 .

Ensaka T . PLL Circuit Design and Application [M ] . He X C, trans. Beijing : China Science Publishing Media Ltd ., 2006 : 31 - 51 .

中华人民共和国国家质量监督检验检疫总局 , 中国国家标准化管理委员会 . 产品几何技术规范（GPS）技术产品文件中表明结构的表示法: GB/T 131—2006 [S ] . 北京 : 中国标准出版社 , 2006 .

General Administration of Quality Supervision , Inspection and Quarantine of the People s Republic of China , Standardization Administration of the People s Republic of China . Geometrical product specification(GPS)-indication of surface texture in technical product documentation : GB/T 131—2006 [S ] . Beijing : Standards Press of China , 2006 .

秦大同 , 谢里阳 . 现代机械设计手册 [M ] . 6版 . 北京 : 化学工业出版社 , 2011 : 225 - 355 .

Qin D T , Xie L Y . Modern Machinery s Handbook [M ] . 6th ed . Beijing : Chemical Industry Press , 2011 : 225 - 355 .

黄志询 . 截止波导理论导论 [M ] . 2版 . 北京 : 中国计量出版社 , 1991 : 111 - 125 .

Huang Z X . An Introduction to the Theory of Waveguide Below Cutoff [M ] . 2nd ed . Beijing : China Metrology Press , 1991 : 111 - 125 .

Russell D H . The waveguide below-cutoff attenuation standard [J ] . IEEE Transactions on Microwave Theory and Techniques , 1997 , 45 ( 12 ): 2408 - 2413 .

Hartel R W . Ice crystallization during the manufacture of ice cream [J ] . Trends in Food Science & Technology , 1996 , 7 ( 10 ): 315 - 321 .

Louis R . Glimpses into the realm of freeze-drying: classical issues and new ventures [M ] // Louis R, Joan C M. Freeze Drying / Lyophilization of Pharmaceutical and Biological Products . 3rd ed . New York : Informa Healthcare , 2010 : 1 - 28 .

Pikal M J , Shah S . The collapse temperature in freeze drying: dependence on measurement methodology and rate of water removal from the glassy phase [J ] . International Journal of Pharmaceutics , 1990 , 62 ( 2 ): 165 - 186 .

Milton N , Pikal M J , Roy M L , et al . Evaluation of manometric temperature measurement as a method of monitoring product temperature during lyophilization [J ] . PDA Journal of Pharmaceutical Science and Technology , 1997 , 51 ( 1 ): 7 - 16 .

Jiang S , Nail S L . Effect of process conditions on recovery of protein activity after freezing and freeze-drying [J ] . European Journal of Pharmaceutics and Biopharmaceutics , 1998 , 45 ( 3 ): 249 - 257 .

王维 , 李强强 , 陈国华 , 等 . 具有初始孔隙的速溶咖啡冷冻干燥实验 [J ] . 农业机械学报 , 2018 , 49 ( 6 ): 347 - 353 .

Wang W , Li Q Q , Chen G H , et al . Experiment on freeze-drying of instant coffee with initial porosity [J ] . Transactions of the Chinese Society for Agricultural Machinery , 2018 , 49 ( 6 ): 347 - 353 .

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