CN101196366B - Low-temperature freeze dryer for experiment - Google Patents
Low-temperature freeze dryer for experiment Download PDFInfo
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- CN101196366B CN101196366B CN200610119313A CN200610119313A CN101196366B CN 101196366 B CN101196366 B CN 101196366B CN 200610119313 A CN200610119313 A CN 200610119313A CN 200610119313 A CN200610119313 A CN 200610119313A CN 101196366 B CN101196366 B CN 101196366B
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Abstract
A low temperature freeze dryer for experiment is provided, which is provided with a freeze chamber on the upper part and a silicon oil bathroom on the lower part; the two rooms are separated by a shelf; the freeze chamber is internally provided with a cold trap coil with one end extending out of barrel wall via the joint of the cold trap coil; the silicon oil bathroom is a cavity with a heating tray arranged on the bottom and silicon oil filled inside to form a silicon oil pool; the shelf is welded with a plurality of pole notches immersed in the silicon oil; the periphery of a shelf platform is welded with a ring shape baffle which forms a ring shape catch basin with the wall of the freeze chamber; a heat exchanger coil is provided in the silicon oil pool with one end extending out of the barrel wall via the joint of the heat exchanger coil and the other end connected with the cold trap coil in the freeze chamber; the inner wall of a liquid nitrogen jar is connected with an electrical heater and the liquid nitrogen exit is directly connected with the cold trap coil or heat exchanger coil through a screwed pipe. A distribution box is separately connected with the electrical heater of the liquid nitrogen jar, a vacuum pump, a PC, the heating tray and a temperature thermocouple of the freeze chamber. The heating tray on the bottom of the silicon oil pool can precisely control the temperature of the silicon oil; the shelf is immersed into the silicon oil pool to take silicon oil bath, thereby being able to realize good heat transfer.
Description
Technical field
The present invention relates to a kind of experiment low-temperature freeze-dry machine, belong to cryogenic vacuum, freeze drying and automatic control technology field.
Background technology
Vacuum Freezing ﹠ Drying Technology is a novel cross discipline that grows up in recent decades, relates to subjects such as heat and mass, refrigeration, vacuum, automatic control.Freeze Drying Technique has been compared many advantages with other drying means: goods are dry at low temperatures, can avoid protein, microorganism and so on generation sex change or lose biologos.This is for the kept dry particularly suitable of heat-sensitive substance such as vaccine, bacterial classification and blood product etc.; Owing to be dry at low temperatures, make the nutrition loss of volatile component in the goods and heated denaturalization very little; In the low temperature drying process, the effect of microbial growth and enzyme almost can't be carried out, and can keep the original proterties of material best; Can keep original shape best after the goods freeze-drying, dry back volume, shape are constant substantially, can be reduced into original shape rapidly after the rehydration; Dry under vacuum, oxygen is few, and the material of easy oxidation is protected; Can remove in the goods about 95% moisture, make its long preservation at room temperature.In view of the good drying effect of Freeze Drying Technique, the freeze-drying that Freeze Drying Technique is applied to tissue of biological cells is preserved, and it is increasingly extensive that medicament preparation becomes, and just becoming new research focus.
Mainly there is following shortcoming in experiment at present with freeze dryer:
Most freeze dryers are to provide cold by cooling cycle system, and rate of temperature fall generally is fixing uncontrollable; The shelf that is used to place frozen goods is dull and stereotyped, can only play heat effect, the slow and effective temperature control of firing rate; Precooling is that material disc is put into cold-trap pre-freeze, and about-45 ℃, minimum can reach-55 ℃ to the temperature of cold-trap, can not satisfy the needs of all kinds of refrigerated products to temperature usually; Need promote or transfer to lucite material bin inner drying when dry, transfer process can make temperature change rapidly, influences the physical characteristic of frozen goods; The required heat of material distillation is by environmental supply etc.
Summary of the invention
The objective of the invention is in order to overcome the current experiments shortcoming of low-temperature freeze-dry machine, a kind of experiment low-temperature freeze-dry machine that can realize the cooling scope of controlled rate of temperature fall, comparatively accurate temperature control uniformly and broadness is provided.
Technical scheme of the present invention is: refrigeration makes it gasification by electric heater heating liquid nitrogen, by the pressure of control gas, extrudes liquid nitrogen as low-temperature receiver; The fore-cooling room adopts the silicone oil pool structure, and heat exchanger adopts the coil pipe that charges into liquid nitrogen, connects a heating plate in bottom, silicone oil pond, regulates compensation by Programmable Logic Controller (PLC) and adds heat, accurately controls the silicone oil temperature; Shelf is the plank frame that is connected with a plurality of post grooves, and special stainless steel shelf immerses in the silicone oil pond can carry out silicone oil bath, realizes the good heat transfer effect; Cold-trap is a spiral coil, is arranged in the cryodesiccation chamber; TT﹠C system is made of jointly upper PC and the next Programmable Logic Controller and data acquisition module, control parameter and monitoring can be set on PC, but every data can be gathered, be stored, upload to temperature curve programme-control, data acquisition module automatically, and data can be handled on PC.
A kind of experiment low-temperature freeze-dry machine comprises cryodesiccation chamber, silicone oil bathroom, cold-trap coil pipe, water storage tank, shelf, silicone oil pond, heat exchanger coils, heating plate, liquid nitrogen container, distribution box, vavuum pump, PC; Be characterized in:
1) top is cryodesiccation chamber, and the bottom is the silicone oil bathroom, and the chamber is separated by shelf up and down;
2) the cold-trap coil pipe is arranged in the cryodesiccation chamber, the cold-trap coil pipe stretches out a barrel wall through cold-trap coil pipe interface;
3) the silicone oil bathroom is a cavity, and the bottom is connected with heating plate, injects silicone oil in it, forms the silicone oil pond; Be connected with a plurality of post grooves on the shelf, the post drill traverse is gone in the silicone oil, periphery at the shelf platform is welded with ring baffle, form annular water storage tank with the freeze-drying locular wall, silicone oil is provided with heat exchanger coils in the pond, the one end stretches out a barrel wall through the heat exchanger coils interface, and the other end is connected with cold-trap coil pipe in the cryodesiccation chamber;
4) the liquid nitrogen container inwall is connected with electric heater; The liquid nitrogen outlet directly is connected with cold-trap coil pipe or heat exchanger coils through screwed pipe;
5) distribution box is connected with the temperature thermocouple of electric heater, vavuum pump, PC, heating plate and the cryodesiccation chamber of liquid nitrogen container respectively.
The present invention does not use the refrigeration machine refrigeration, and is to use liquid nitrogen as low-temperature receiver, and by the built-in electric heater heating liquid nitrogen of liquid nitrogen container, the pressure of gas extrudes liquid nitrogen in the control liquid nitrogen container.Liquid nitrogen is forced out the back and flows into silicone oil pond heat exchanger coils, carries out heat exchange with silicone oil, controls the temperature of shelf by control silicone oil temperature.
The precooling stage is supplied with interface with liquid nitrogen and is connected with silicone oil pond heat exchanger coils interface earlier, allows liquid nitrogen flow into silicone oil pond heat exchanger coils earlier, flows into the cold-trap coil pipe then; The lyophilization stage, liquid nitrogen is supplied with interface be connected with cold-trap coil pipe interface earlier, allow liquid nitrogen flow into the cold-trap coil pipe earlier, flow into silicone oil pond heat exchanger coils then, can effectively reduce the liquid nitrogen consumption.
Arrange heating plate in bottom, silicone oil pond, regulate compensation by Programmable Logic Controller (PLC) and add heat, thus the temperature of control silicone oil.
Special stainless steel shelf immerses in the silicone oil pond and carries out silicone oil bath, can realize good heat transfer.
TT﹠C system is made of jointly upper PC and the next Programmable Logic Controller and data acquisition module, control parameter and monitoring can be set on PC, but temperature curve programme-control, every data can be gathered, be stored, upload to data acquisition module automatically, and all data all can be handled on PC.
A kind of beneficial effect of testing with the low-temperature freeze-dry machine of the present invention is: but because the programme-control of heating plate temperature, the silicone oil temperature can accurately be controlled, because the post groove that shelf connects down immerses in the silicone oil fully, shelf temperature is evenly distributed, can control as required, control accuracy is 0.1 ℃, and low energy drops to-100 ℃; Vacuum is lower than 15Pa.Condenser temperature can be controlled as required, and minimum reaching-115 ℃ can be satisfied cell, biological products and medicine freeze-drying experimental requirements.
Description of drawings
Fig. 1 is a kind of overall structure schematic diagram of testing with the low-temperature freeze-dry machine of the present invention;
Fig. 2 is the structural representation of shelf of the present invention.
1. cryodesiccation chamber, 2. cold-trap coil pipe, 3. water storage tank, 4. shelf, 5. silicone oil pond, 6. heat exchanger coils, 7. heating plate, 8. liquid nitrogen container, 9. distribution box, 10. vavuum pump, 11.PC machine, 12. cold-trap coil pipe interfaces, 13. heat exchanger coils interfaces, 14. post grooves, 15. liquid nitrogen are supplied with interface
The specific embodiment
A kind of experiment of the present invention low-temperature freeze-dry machine, top is cryodesiccation chamber 1, the bottom is the silicone oil bathroom, is separated by shelf 4 between two Room; Cold-trap coil pipe 2 is arranged in the cryodesiccation chamber, and the cold-trap coil pipe interface 12 of cold-trap coil pipe on the freeze-drying locular wall stretches out a barrel wall; The silicone oil bathroom is a cavity, and the bottom is connected with heating plate 7 (2KW), injects silicone oil in it, forms silicone oil pond 5; Be connected with a plurality of post grooves 14 on the shelf 4, the post drill traverse is gone in the silicone oil, periphery at the shelf platform is welded with ring baffle, form annular water storage tank 3 with the freeze-drying locular wall, be provided with heat exchanger coils 6 in the silicone oil pond, the one end stretches out a barrel wall through heat exchanger coils interface 13, and the other end is connected with cold-trap coil pipe 2 in the cryodesiccation chamber; Liquid nitrogen container 8 inwalls are connected with electric heater; Liquid nitrogen outlet directly is connected with cold-trap coil pipe 2 or heat exchanger coils 6 through screwed pipe. and distribution box 9 is connected with the temperature thermocouple of electric heater, vavuum pump 10, PC 11, heating plate 7 and the cryodesiccation chamber of liquid nitrogen container 8 respectively.
The sample that needs freeze-drying is placed in the post groove 14 of shelf 4, post groove the inside is filled some silicone grease earlier, and the rotation bottle fully contacts it with the post cell wall.Post groove middle part and bottom are arranged two thermocouples respectively, arrange a thermocouple in the suspension, thermocouple in the post exterior silicone oil pond 5, and layout thermocouple in cold-trap coil pipe 2 walls middle part is used for the variations in temperature of each measuring point in the monitoring record freeze-drying process.
At first fix top gland, liquid nitrogen is supplied with interface 15 be connected with heat exchanger coils interface 13, opening power, the operation control program configures each parameter, opens whole system.After pre-freeze is finished, liquid nitrogen is supplied with interface 15 be connected with cold-trap coil pipe interface 12 earlier, open vavuum pump, begin to enter the lyophilization process.During lyophilization the silicone oil temperature is controlled at required primary drying temperature, after material temperature equates with the temperature of post trench bottom and keeps a period of time, shelf 4 temperature is set in required redrying temperature, begin to enter the adsorption stripping and dry stage.Invariable when material temperature, whole dry run finishes.Open vent valve, open cryodesiccation chamber, the freeze-dried products vacuum seal bag of packing into is rapidly stored.
The test example:
Usually the method for the permanent preservation employing of Cord blood is to drop in the liquid nitrogen behind the programmed cooling to preserve, and such preserving type costs an arm and a leg, and energy consumption is big.People attempt preserving Cord blood for a long time with the method for freeze-drying now.Before this, doctor Xiao Honghai etc. have carried out preliminary experimental study to the karyocyte that separates in the bleeding of the umbilicus first, and recording the high viability of karyocyte is 55.7%.Here use the low-temperature freeze-dry machine of development newly that the Cord blood whole blood is carried out preliminary freeze-drying research.
The cell suspension bottle for preparing is placed in the post groove 14 of shelf 4, post groove the inside is filled some silicone grease earlier, and the rotation bottle fully contacts it with the pillar wall.Post groove middle part and bottom are arranged two thermocouples respectively, arrange a thermocouple in the suspension, thermocouple in the outside silicone oil of the post groove pond 5, and layout thermocouple in cold-trap coil pipe 2 walls middle part is used for the variations in temperature of each measuring point in the monitoring record freeze-drying process.
Precooling stage freeze-drying suspension rate of temperature fall is-2.1 ℃/min, and whole freezing process continues about 1 hour, and freeze-drying this moment suspension temperature drops to-100 ℃.After pre-freeze was finished, condenser temperature was controlled between-60 ℃～-50 ℃, opened vavuum pump 10, began to enter lyophilization.In the primary drying stage, be controlled at-40 ℃ with the silicone oil temperature this moment, after material temperature equates with the temperature of post trench bottom and keeps a period of time, shelf 4 temperature is set in 20 ℃, begins to enter the adsorption stripping and dry stage.Invariable when material temperature, whole dry run finishes.The precooling stage, the rate of temperature fall of suspension and to freeze whole temperature be crucial, the more common freeze dryer of rate of temperature fall wants fast here, and suspension freezes eventually that temperature is-100 ℃, can realize the segment glass transformation of suspension, and the damage of pair cell is less; Primary drying begins, and the temperature of suspension raises with the temperature of shelf, and the devitrification crystallization may take place, and this can cause damage by pair cell, but the time that this process continues is shorter; Whole process cold-trap temperature when adding liquid nitrogen has fluctuation, but influence is not too big to material.
Utilizing this equipment that the human cord blood whole blood has been carried out the vacuum freeze-drying experiment, is that the karyocyte recovery rate can reach 71.1% after the Cord blood whole blood freeze-drying rehydration of 40% a polyethylene pyrrolidone (W/W)+10% trehalose (W/W)+10% sweet mellow wine (W/W) with protective agent.
Claims (1)
1. an experiment low-temperature freeze-dry machine comprises cryodesiccation chamber, silicone oil bathroom, cold-trap coil pipe, water storage tank, shelf, silicone oil pond, heat exchanger coils, heating plate, liquid nitrogen container, distribution box, vavuum pump, PC; It is characterized in that:
1) top is cryodesiccation chamber, and the bottom is the silicone oil bathroom, and upper and lower chamber is separated by shelf;
2) the cold-trap coil pipe is arranged in the cryodesiccation chamber, the cold-trap coil pipe stretches out a barrel wall through cold-trap coil pipe interface;
3) the silicone oil bathroom is a cavity, and the bottom is connected with heating plate, injects silicone oil in it, forms the silicone oil pond; Be connected with a plurality of post grooves on the shelf, the post drill traverse is gone in the silicone oil, periphery at the shelf platform is welded with ring baffle, form annular water storage tank with the freeze-drying locular wall, silicone oil is provided with heat exchanger coils in the pond, the one end stretches out a barrel wall through the heat exchanger coils interface, and the other end is connected with cold-trap coil pipe in the cryodesiccation chamber;
4) the liquid nitrogen container inwall is connected with electric heater; The liquid nitrogen outlet directly is connected with cold-trap coil pipe or heat exchanger coils through screwed pipe;
5) distribution box is connected with the temperature thermocouple of electric heater, vavuum pump, PC, heating plate and the cryodesiccation chamber of liquid nitrogen container respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610119313A CN101196366B (en) | 2006-12-07 | 2006-12-07 | Low-temperature freeze dryer for experiment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200610119313A CN101196366B (en) | 2006-12-07 | 2006-12-07 | Low-temperature freeze dryer for experiment |
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| CN101196366A CN101196366A (en) | 2008-06-11 |
| CN101196366B true CN101196366B (en) | 2010-05-12 |
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| CN200610119313A Expired - Fee Related CN101196366B (en) | 2006-12-07 | 2006-12-07 | Low-temperature freeze dryer for experiment |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008153039A1 (en) * | 2007-06-14 | 2008-12-18 | Ulvac, Inc. | Vacuum freeze-drying apparatus and method of vacuum freeze drying |
| CN102089606B (en) * | 2008-07-10 | 2013-07-10 | 株式会社爱发科 | Freeze-drying device |
| CN104785311A (en) * | 2015-03-09 | 2015-07-22 | 韩山师范学院 | Experimental type liquid nitrogen quick freezing simple device |
| CN107782860A (en) * | 2017-12-06 | 2018-03-09 | 苏州市苏测检测技术有限公司 | Array food samples quality quick detection mechanism |
| CN108955098B (en) * | 2018-08-16 | 2023-09-15 | 中国科学院理化技术研究所 | Low-temperature system integrating constant temperature, cooling and vacuum freeze-drying |
| CN111998616A (en) * | 2020-07-16 | 2020-11-27 | 广州蓝日生物科技有限公司 | Sublimation dewatering device |
| CN114353440B (en) * | 2021-12-23 | 2023-06-16 | 青岛海尔生物医疗股份有限公司 | Control method and device for freeze dryer and freeze dryer |
| CN114688834A (en) * | 2022-03-15 | 2022-07-01 | 青海省地方病预防控制所 | Freeze-drying preparation method of plague FI antibody diagnostic product |
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| US4501719A (en) * | 1981-05-04 | 1985-02-26 | Marquest Medical Products, Inc. | Tray apparatus for freeze-drying biologicals having a predetermined unit dosage |
| EP0864071A1 (en) * | 1995-11-29 | 1998-09-16 | IMMUNO Aktiengesellschaft | Lyophilization method and device, containers and filling systems |
| CN2352909Y (en) * | 1998-08-28 | 1999-12-08 | 张祯儒 | Freezing type drying machine |
| WO2001079773A1 (en) * | 2000-04-19 | 2001-10-25 | Astrazeneca Ab | Method of monitoring a freeze drying process |
| CN2651678Y (en) * | 2003-06-26 | 2004-10-27 | 上海俊乐制冷自控元件有限公司 | Multifunctional experimental refrigerating drier |
| CN2757071Y (en) * | 2004-12-15 | 2006-02-08 | 上海远东制药机械总厂 | Freeze-drying machine partition board |
| CN200989866Y (en) * | 2006-12-07 | 2007-12-12 | 上海理工大学 | Cryogenic freeze dryer for biological medical experiment |
-
2006
- 2006-12-07 CN CN200610119313A patent/CN101196366B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4501719A (en) * | 1981-05-04 | 1985-02-26 | Marquest Medical Products, Inc. | Tray apparatus for freeze-drying biologicals having a predetermined unit dosage |
| EP0864071A1 (en) * | 1995-11-29 | 1998-09-16 | IMMUNO Aktiengesellschaft | Lyophilization method and device, containers and filling systems |
| CN2352909Y (en) * | 1998-08-28 | 1999-12-08 | 张祯儒 | Freezing type drying machine |
| WO2001079773A1 (en) * | 2000-04-19 | 2001-10-25 | Astrazeneca Ab | Method of monitoring a freeze drying process |
| CN2651678Y (en) * | 2003-06-26 | 2004-10-27 | 上海俊乐制冷自控元件有限公司 | Multifunctional experimental refrigerating drier |
| CN2757071Y (en) * | 2004-12-15 | 2006-02-08 | 上海远东制药机械总厂 | Freeze-drying machine partition board |
| CN200989866Y (en) * | 2006-12-07 | 2007-12-12 | 上海理工大学 | Cryogenic freeze dryer for biological medical experiment |
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Granted publication date: 20100512 Termination date: 20121207 |