CN101793458A - 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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- CN101793458A CN101793458A CN 201010144170 CN201010144170A CN101793458A CN 101793458 A CN101793458 A CN 101793458A CN 201010144170 CN201010144170 CN 201010144170 CN 201010144170 A CN201010144170 A CN 201010144170A CN 101793458 A CN101793458 A CN 101793458A
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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
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- 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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- General Engineering & Computer Science (AREA)
- Drying Of Solid Materials (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a vacuum freezing drying device with functions of DSC and microstructure observation, which consists of a freezing drying system, a vacuum system, a DSC thermal analysis system, a micro imaging system, a residual moisture measurement system and a computer. The freezing drying system comprises a freezing drying chamber, a heating device and a refrigeration device, wherein the freezing drying chamber is a closed container, a transparent part is arranged on the wall of the container, and the heating device and the refrigeration device are arranged on the freezing drying chamber. The DSC thermal analysis system and the residual moisture measurement system are arranged in the freezing drying chamber; the micro imaging system is arranged outside the freezing drying chamber; and each system is connected with the computer respectively. The vacuum freezing drying device is suitable for the freezing drying research on biological products, medicaments and other thermosensitive substances, and can not only measure the thermal effect of the freezing system and analyze the pre-freezing quality by using the DSC thermal analysis function at the pre-freezing stage, but also observe ice crystal formation dimension and ice crystal sublimation condition in real time in the freezing drying system through the micro imaging system at the sublimation drying stage.
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 will contain water freezes 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 to make its sex change owing to temperature is too high when producing, 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 practice, the thickness of bottled material and bottleneck size can be comparable, and it radially conducts heat the influence of freeze-drying process be can not ignore.In addition, the influence factor of freeze-drying process is more and interrelated, freeze-drying parameter and technology that the method that therefore can only study by experiment obtains to suit.
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 of normal employing are differential scanning calorimetry (DSC), this method can be measured the difference of temperature changing process between sample and the sensor probe, 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 provide more efficiently reference and guidance, 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; Described 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 outdoor, 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, by 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, described 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 dry indoor sample is lowered the temperature with freezing with this.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, described 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, described heater element comprises electrical heating wire and temperature controller.Electrical heating wire evenly is installed in the hothouse container outer surface, regulates heating power by 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, described 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, described DSC TAS is made up of sample platform and reference platform, and is fixed by bolts to by securing member on the bottom of freeze drying chamber.
In above-mentioned vacuum freezing drying device with DSC and microstructure observation, described 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 described sample platform 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, described 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, described 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 by 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.
Described 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 sliding when operation.。Described 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 be connected with temperature controller 7, in temperature-fall period, also need freeze drying chamber 1 is carried out temperature control, therefore at the container outer surface uniform winding electrical heating wire 6 of freeze drying chamber 1, this electrical heating wire 6 is by temperature controller 7 controls, regulate heating power 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.Described refrigeration device comprises heat conductive bar 3 and liquid nitrogen 5, heat conductive bar 3 and liquid nitrogen 5 all are located under the support 2, 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 sample in the freeze drying chamber 1 is lowered the temperature and freezing with this.Described 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; Described DSC TAS is made up of sample platform 18 and reference platform 19, and is fixed by bolts to by securing member 21 on the bottom of freeze drying chamber 1.Be separately installed with temperature thermocouple line 20 on described sample platform 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 platform, just can detect sample platform this temperature changing process with respect to reference platform by the temperature thermocouple line 20 on the sample platform this moment, and data are presented on the moisture recorder, transfer to then and carry out data in the computer 13 and preserve.
The residual moisture measuring system is located at freeze drying chamber 1 inside; Described 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 by data wire 24 with transfer of data to the 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)
1. the vacuum freezing drying device that has DSC and microstructure observation is characterized in that being made up of lyophilization system, vacuum system, DSC TAS, microscope camera system, residual moisture measuring system and computer; Described 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 outdoor, 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, by 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.
2. according to the described vacuum freezing drying device of claim 1, it is characterized in that described freeze drying is indoor to be provided with a plurality of sample cells with DSC and microstructure observation.
3. according to the described vacuum freezing drying device of claim 1, it is characterized in that described DSC TAS is made up of sample platform and reference platform, and be fixed on by securing member on the bottom of freeze drying chamber with DSC and microstructure observation.
4. according to the described vacuum freezing drying device of claim 1, it is characterized in that described vacuum system comprises vacuum pipe, vavuum pump, hand-operated valve, vacuum meter and atmospheric valve with DSC and microstructure observation; 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.
5. according to the described vacuum freezing drying device of claim 3 with DSC and microstructure observation, it is characterized in that being separately installed with the temperature thermocouple line on described sample platform and the reference platform, the temperature thermocouple line connects moisture recorder, and moisture recorder connects computer again.
6. according to the described vacuum freezing drying device of claim 1, it is characterized in that described chamber wall is provided with transparent part and is meant that freeze drying chamber adopts transparent seal cover with DSC and microstructure observation.
7. according to the described vacuum freezing drying device of claim 1, it is characterized in that described residual moisture measuring system is meant humidity sensor with DSC and microstructure observation.
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 |
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| Publication Number | Publication Date |
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| CN101793458A true CN101793458A (en) | 2010-08-04 |
| CN101793458B CN101793458B (en) | 2012-03-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010101441709A Expired - Fee Related CN101793458B (en) | 2010-04-02 | 2010-04-02 | Vacuum freezing drying device with functions of DSC and microstructure observation |
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| Country | Link |
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| CN (1) | CN101793458B (en) |
| WO (1) | WO2011120342A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011120342A1 (en) * | 2010-04-02 | 2011-10-06 | 中山大学 | Vacuum freeze-drying apparatus |
| WO2015024141A1 (en) * | 2013-08-22 | 2015-02-26 | 国玺干细胞应用技术股份有限公司 | Biological product storage device provided with observation element |
| WO2019085734A1 (en) * | 2017-10-31 | 2019-05-09 | 王一田 | Steam pasteurization method for freeze-dried food |
| CN110057821A (en) * | 2019-04-16 | 2019-07-26 | 上海交通大学 | Cryo-microscope imaging system for mankind's gamete fast freeze-thaw process observation |
| CN110132791A (en) * | 2019-05-17 | 2019-08-16 | 杭州仰仪科技有限公司 | Liquid cryogen fluidity testing conduction cooling vibration isolation sample container |
| 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 |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2551687A (en) * | 2016-03-04 | 2018-01-03 | Linkam Scient Instruments Ltd | Freeze drying apparatus |
| CN110108690B (en) * | 2019-06-10 | 2023-11-24 | 中国科学院生物物理研究所 | Ultralow-temperature sample-changeable microscopic imaging system and working method thereof |
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| CN1818738A (en) * | 2006-03-10 | 2006-08-16 | 浙江大学 | Microscope observation system during freezing dry process |
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| CN201615678U (en) * | 2010-04-02 | 2010-10-27 | 中山大学 | Vacuum freeze drying device with DSC and microstructure observation functions |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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
-
2011
- 2011-01-11 WO PCT/CN2011/070189 patent/WO2011120342A1/en active Application Filing
Patent Citations (5)
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| JPH09229884A (en) * | 1996-02-21 | 1997-09-05 | Shimadzu Corp | Thermal analysis apparatus |
| CN1818738A (en) * | 2006-03-10 | 2006-08-16 | 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 |
| CN201387412Y (en) * | 2009-03-24 | 2010-01-20 | 山西农业大学 | Water content online monitoring device during freeze drying process of fresh products |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011120342A1 (en) * | 2010-04-02 | 2011-10-06 | 中山大学 | Vacuum freeze-drying apparatus |
| WO2015024141A1 (en) * | 2013-08-22 | 2015-02-26 | 国玺干细胞应用技术股份有限公司 | Biological product storage device provided with observation element |
| WO2019085734A1 (en) * | 2017-10-31 | 2019-05-09 | 王一田 | Steam pasteurization method for freeze-dried food |
| US10849341B2 (en) | 2017-10-31 | 2020-12-01 | Yitian Wang | Steam pasteurization method for freeze-dried food |
| CN110057821A (en) * | 2019-04-16 | 2019-07-26 | 上海交通大学 | Cryo-microscope imaging system for mankind's gamete fast freeze-thaw process observation |
| CN110132791A (en) * | 2019-05-17 | 2019-08-16 | 杭州仰仪科技有限公司 | Liquid cryogen fluidity testing conduction cooling vibration isolation sample container |
| 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 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101793458B (en) | 2012-03-21 |
| WO2011120342A1 (en) | 2011-10-06 |
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