CN101793458B - Vacuum freezing drying device with functions of DSC and microstructure observation - Google Patents
Vacuum freezing drying device with functions of DSC and microstructure observation Download PDFInfo
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- CN101793458B CN101793458B CN2010101441709A CN201010144170A CN101793458B CN 101793458 B CN101793458 B CN 101793458B CN 2010101441709 A CN2010101441709 A CN 2010101441709A CN 201010144170 A CN201010144170 A CN 201010144170A CN 101793458 B CN101793458 B CN 101793458B
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- 238000007710 freezing Methods 0.000 title abstract description 26
- 230000008014 freezing Effects 0.000 title abstract description 26
- 238000001035 drying Methods 0.000 title abstract description 21
- 238000004108 freeze drying Methods 0.000 claims abstract description 90
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 10
- 238000002076 thermal analysis method Methods 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 2
- 238000005057 refrigeration Methods 0.000 abstract description 7
- 239000003814 drug Substances 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 2
- 230000008022 sublimation Effects 0.000 abstract 2
- 238000000859 sublimation Methods 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 24
- 239000000523 sample Substances 0.000 description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 238000000034 method Methods 0.000 description 12
- 239000007788 liquid Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 230000008569 process Effects 0.000 description 8
- 238000012546 transfer Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4846—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample
- G01N25/4866—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample by using a differential method
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/0332—Cuvette constructions with temperature control
- G01N2021/0335—Refrigeration of cells; Cold stages
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Biochemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Drying Of Solid Materials (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
本发明公开了具有DSC及微结构观察功能的真空冷冻干燥装置，由冷冻干燥系统、真空系统、DSC热分析系统、显微摄像系统、残余水分测量系统和计算机组成；冷冻干燥系统包括冷冻干燥室、加热器件和制冷器件，冷冻干燥室为一密闭容器，容器壁上设有透明部分，加热器件和制冷器件设于冷冻干燥室上；DSC热分析系统和残余水分测量系统设于冷冻干燥室内部；显微摄像系统设于冷冻干燥室外部；各个系统分别与计算机连接。本发明适用于生物制品、药品等热敏性物质的冷冻干燥研究，不仅能够在预冻阶段利用DSC热分析功能测量冷冻体系的热效应并分析预冻质量，还能够在升华干燥阶段通过显微摄像系统实时观察冻干体系中冰晶形成大小和冰晶升华情况。
The invention discloses a vacuum freeze-drying device with DSC and microstructure observation functions, which is composed of a freeze-drying system, a vacuum system, a DSC thermal analysis system, a microscopic camera system, a residual moisture measurement system and a computer; the freeze-drying system includes a freeze-drying chamber , heating device and refrigeration device, the freeze-drying chamber is a closed container with a transparent part on the container wall, the heating device and refrigeration device are arranged on the freeze-drying chamber; the DSC thermal analysis system and the residual moisture measurement system are arranged inside the freeze-drying chamber ; The micro camera system is located outside the freeze-drying chamber; each system is connected with the computer respectively. The invention is applicable to the freeze-drying research of heat-sensitive substances such as biological products and medicines. It can not only use the DSC thermal analysis function to measure the thermal effect of the freezing system and analyze the pre-freezing quality in the pre-freezing stage, but also can use the microscopic camera system in the sublimation drying stage. Observe the ice crystal formation size and ice crystal sublimation in the freeze-drying system.
Description
Technical field
The present invention relates to a kind of vacuum freezing drying device, specifically, relate to the vacuum freezing drying device of a kind of DSC of having and microstructure observation.
Background technology
Vacuum freeze drying is that the material that contains water is freezed to form ice at low temperatures, under vacuum condition, frozen materials is heated then, makes the ice distillation, thereby obtains a kind of drying means of dried product.For heat-sensitive substances such as biological products, medicines, in order to prevent when producing, to make its sex change owing to temperature is too high, Vacuum Freezing & Drying Technology is undoubtedly ideal production and processing method.The biological products of freeze-drying, medicine generally all are made into injection, for the convenience of its storage and use, adopt the form of bottled material freeze-drying usually.
Freeze dryer is the normal device that adopts of vacuum freeze drying; Because the contact area of its heated barrier and bottled material is little; Feasible heat transfer often becomes the major control step of freeze-drying process, and the one dimensional heat transfer model that move at the bottom of bottle equably at the distillation interface becomes the main model that instructs of testing and producing.The heat that the one dimensional heat transfer model has been ignored the bottle side imports into, yet in reality, the thickness of bottled material can be compared with the bottleneck size mutually, and it radially conducts heat the influence of freeze-drying process can not ignore.In addition, the influence factor of freeze-drying process is more and interrelated, the freeze-drying parameter and the technology that therefore can only obtain to suit through the method for experimental study.
Successful freeze-drying process not only depends on the structure cognizing of freeze-drying prods, also depends on heat, the dynamic process of freeze-drying.Wherein, The structural research and the thermoanalytical method that the most often adopt are differential scanning calorimetry (DSC); This method can measuring samples and sensor probe between the difference of temperature changing process; Its thermal behavior goes on record, according to the record the DSC curve, can analyze the freeze-drying sample freezing point, freeze characteristic and glass transition characteristic.In addition, microscope is a kind of structural research method the most intuitively, and it can observe directly the microstructure of sample.
In order in depth to study and obtain to have the data of practical value comprehensively to the freeze drying of heat-sensitive substances such as bottled biological products, medicine; So that more efficiently reference and guidance are provided, need a kind of vacuum freezing drying device with DSC and microstructure observation to its actual production.
Summary of the invention
The object of the present invention is to provide and a kind ofly can measure the vacuum freezing drying device of freeze-drying sample fuel factor and structural change in real time.
To achieve these goals, the present invention adopts following technical scheme:
A kind of vacuum freezing drying device with DSC and microstructure observation is made up of lyophilization system, vacuum system, DSC TAS, microscope camera system, residual moisture measuring system and computer; Said lyophilization system comprises freeze drying chamber, heater element and refrigeration device, and freeze drying chamber is a closed container, and chamber wall is provided with transparent part, and heater element and refrigeration device are located on the freeze drying chamber; Freeze drying chamber connects vacuum system; The DSC TAS is located at the freeze drying chamber interior; Microscope camera system is located at the freeze drying outside, and the transparent part that can see through on the freeze drying locular wall is observed the inner sample microstructure; The residual moisture measuring system is located at the freeze drying chamber interior, through measuring the indoor steam dividing potential drop of freeze drying to measure the residual moisture content of freeze-dried material; DSC TAS, microscope camera system and residual moisture measuring system are connected with computer respectively.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation; Said refrigeration device comprises heat conductive bar and liquid nitrogen; The bottom of freeze drying chamber is connected with heat conductive bar one end; The other end of heat conductive bar immerses in the liquid nitrogen, thereby cold is reached hothouse, and with this dry indoor sample is lowered the temperature with freezing.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, said liquid nitrogen is located on the lifting platform.The degree of depth that heat conductive bar immerses in the liquid nitrogen can be passed through the lifting platform free adjustment.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, said heater element comprises electrical heating wire and temperature controller.Electrical heating wire evenly is installed in the hothouse container outer surface, regulates heating power through temperature controller according to the temperature program(me) of setting, for the indoor sample of freeze drying provides thermal source.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, said freeze drying is indoor to be provided with a plurality of sample cells, can place a plurality of bottled samples.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, said DSC TAS is made up of sample stage and reference platform, and is fixed by bolts on the bottom of freeze drying chamber through securing member.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, said vacuum system comprises vacuum pipe, vavuum pump, hand-operated valve, vacuum meter and atmospheric valve; Vacuum pipe has two, is connected with freeze drying chamber respectively; Be connected with vavuum pump, hand-operated valve and vacuum meter on the vacuum pipe that freeze drying chamber is connected, be connected with atmospheric valve on another vacuum pipe that is connected with freeze drying chamber.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, be separately installed with the temperature thermocouple line on said sample stage and the reference platform, the temperature thermocouple line connects moisture recorder, and moisture recorder connects computer again.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, said chamber wall is provided with transparent part and is meant that freeze drying chamber adopts transparent seal cover.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, said residual moisture measuring system is meant humidity sensor.
Compared with prior art; The present invention has following beneficial effect: freeze drying plant of the present invention is applicable to the freeze drying research of heat-sensitive substances such as biological products, medicine; Not only can utilize the DSC function of thermal analysis to measure the fuel factor of freezing system and analyze the pre-freeze quality in the pre-freeze stage; Can also the lyophilization stage through microscope camera system Real Time Observation freeze-drying system in ice crystal form size and the ice crystal situation that distils, for the Freeze Drying Technique of heat-sensitive substances such as biological products, medicine provides a kind of comprehensive research platform.
Description of drawings
Fig. 1 is the vacuum freezing drying device structural representation that embodiment 1 has DSC and microstructure observation.
Fig. 2 is the freeze drying chamber structural representation of embodiment 1.
The specific embodiment
As depicted in figs. 1 and 2, have the vacuum freezing drying device of DSC and microstructure observation, form by lyophilization system, vacuum system, DSC TAS, microscope camera system, residual moisture measuring system and computer.
Said lyophilization system comprises freeze drying chamber 1, heater element and refrigeration device.Freeze drying chamber 1 is a closed container, adopts transparent seal cover 17 on the chamber wall, and freeze drying chamber 1 is fixed on the support 2, avoids when operation, sliding.。Said heater element comprises electrical heating wire 6 and temperature controller 7; Electrical heating wire 6 is wrapped in freeze drying chamber 1 outer surface, and is connected with temperature controller 7, in temperature-fall period; Also need carry out temperature control to freeze drying chamber 1; Therefore at the container outer surface uniform winding electrical heating wire 6 of freeze drying chamber 1, this electrical heating wire 6 is regulated heating power through temperature controller 7 controls according to the temperature program(me) of setting; Thereby consume too much cold, to realize heating or thermostatic control to sample in the freeze drying chamber 1 by the liquid nitrogen input.Be provided with a plurality of sample cells 22 in the freeze drying chamber 1, bottled sample to be detected just is located in the sample cell 22.Said refrigeration device comprises heat conductive bar 3 and liquid nitrogen 5; Heat conductive bar 3 all is located under the support 2 with liquid nitrogen 5; The bottom of freeze drying chamber 1 is connected with heat conductive bar 3 one ends; The other end of heat conductive bar 3 immerses in the liquid nitrogen 5, cold being reached freeze drying chamber 1, and with this sample in freeze drying chamber 1 is lowered the temperature with freezing.Said liquid nitrogen 5 is located on the lifting platform 4, and the degree of depth that heat conductive bar 3 immerses in the liquid nitrogen 5 can be passed through lifting platform 4 free adjustment.
The DSC TAS is located at freeze drying chamber 1 inside; Said DSC TAS is made up of sample stage 18 and reference platform 19, and is fixed by bolts on the bottom of freeze drying chamber 1 through securing member 21.Be separately installed with temperature thermocouple line 20 on said sample stage 18 and the reference platform 19, temperature thermocouple line 20 passes freeze drying chamber 1 and connects moisture recorder 14, and moisture recorder 14 connects computer 13 again.When sample when pre-freeze stage and lyophilization stage undergo phase transition crystallization and ice crystal distillation; Can produce the release of heat and the variation of thermal capacitance; Thereby cause the variation of local temperature on the sample stage; Just can detect sample stage this temperature changing process with respect to reference platform through the temperature thermocouple line 20 on the sample stage this moment, and data are presented on the moisture recorder, transfers to then to carry out the data preservation in the computer 13.
The residual moisture measuring system is located at freeze drying chamber 1 inside; Said residual moisture measuring system is meant humidity sensor 23; Steam dividing potential drop in the humidity sensor 23 energy measurement freeze drying chambers 1; And pass through data wire 24 with transfer of data to humidity display instrument; Deposit computer 13 then in, change according to the steam dividing potential drop in the freeze drying chamber 1 at last, can calculate the change in concentration of residual moisture in the freeze-dried material.
Claims (7)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101441709A CN101793458B (en) | 2010-04-02 | 2010-04-02 | Vacuum freezing drying device with functions of DSC and microstructure observation |
| PCT/CN2011/070189 WO2011120342A1 (en) | 2010-04-02 | 2011-01-11 | Vacuum freeze-drying apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101441709A CN101793458B (en) | 2010-04-02 | 2010-04-02 | Vacuum freezing drying device with functions of DSC and microstructure observation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101793458A CN101793458A (en) | 2010-08-04 |
| CN101793458B true CN101793458B (en) | 2012-03-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101441709A Expired - Fee Related CN101793458B (en) | 2010-04-02 | 2010-04-02 | Vacuum freezing drying device with functions of DSC and microstructure observation |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN101793458B (en) |
| WO (1) | WO2011120342A1 (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793458B (en) * | 2010-04-02 | 2012-03-21 | 中山大学 | Vacuum freezing drying device with functions of DSC and microstructure observation |
| CN105263817B (en) * | 2013-08-22 | 2017-04-12 | 国玺干细胞应用技术股份有限公司 | Biological product storage device with observation element |
| GB2551687A (en) * | 2016-03-04 | 2018-01-03 | Linkam Scient Instruments Ltd | Freeze drying apparatus |
| CN107568558B (en) | 2017-10-31 | 2021-02-02 | 王一田 | Steam pasteurization method of freeze-dried food |
| CN110057821B (en) * | 2019-04-16 | 2021-09-07 | 上海交通大学 | A cryomicroscopy imaging system for observation of rapid freezing and thawing of human gametes |
| CN110132791B (en) * | 2019-05-17 | 2021-11-26 | 杭州仰仪科技有限公司 | Cold-conducting vibration-isolating sample container for testing low-temperature fluidity of liquid |
| CN110108690B (en) * | 2019-06-10 | 2023-11-24 | 中国科学院生物物理研究所 | An ultra-low temperature replaceable sample microscopy imaging system and its working method |
| CN110530925A (en) * | 2019-08-08 | 2019-12-03 | 西安交通大学 | A kind of DSC heat analysis method applying electric field action |
| US12085337B2 (en) | 2021-10-20 | 2024-09-10 | DSM Sales & Manufacturing, Inc. | Freeze-drying systems and methods |
| CN114544317A (en) * | 2022-02-23 | 2022-05-27 | 上海少卿白鞘医疗科技有限公司 | Freeze thawing instrument for cell detection |
| CN119475823B (en) * | 2025-01-14 | 2025-04-15 | 中国农业科学院农产品加工研究所 | Heat transfer simulation method, system, device and medium for material freezing process |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH09229884A (en) * | 1996-02-21 | 1997-09-05 | Shimadzu Corp | Thermal analyzer |
| CN100346190C (en) * | 2006-03-10 | 2007-10-31 | 浙江大学 | Microscope observation system during freezing dry process |
| CN201083735Y (en) * | 2007-06-26 | 2008-07-09 | 上海理工大学 | Low-temperature microscopic differential scanning calorimetry system main apparatus |
| CN101419015B (en) * | 2008-09-02 | 2010-12-22 | 上海理工大学 | Method for judging once lyophilization drying end point and secondary drying end point |
| CN201387412Y (en) * | 2009-03-24 | 2010-01-20 | 山西农业大学 | On-line moisture monitoring device for fruits and vegetables during freeze-drying process |
| CN201615678U (en) * | 2010-04-02 | 2010-10-27 | 中山大学 | Vacuum freeze-drying device with DSC and microstructure observation function |
| CN101793458B (en) * | 2010-04-02 | 2012-03-21 | 中山大学 | Vacuum freezing drying device with functions of DSC and microstructure observation |
-
2010
- 2010-04-02 CN CN2010101441709A patent/CN101793458B/en not_active Expired - Fee Related
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2011
- 2011-01-11 WO PCT/CN2011/070189 patent/WO2011120342A1/en active Application Filing
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| Publication number | Publication date |
|---|---|
| WO2011120342A1 (en) | 2011-10-06 |
| CN101793458A (en) | 2010-08-04 |
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