CN2888373Y - Freezing-drying machine with liquid nitrogen to assist refrigerate - Google Patents
Freezing-drying machine with liquid nitrogen to assist refrigerate Download PDFInfo
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- CN2888373Y CN2888373Y CN 200520046351 CN200520046351U CN2888373Y CN 2888373 Y CN2888373 Y CN 2888373Y CN 200520046351 CN200520046351 CN 200520046351 CN 200520046351 U CN200520046351 U CN 200520046351U CN 2888373 Y CN2888373 Y CN 2888373Y
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- liquid nitrogen
- trap
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Abstract
The utility model relates to a liquid nitrogen-aided refrigeration freeze-dryer, comprising a vacuum pump, a set of mechanical refrigerating unit, a conventional cold trap and a freeze drying chamber. The conventional cold trap is connected respectively with the vacuum pump, the set of mechanical refrigerating unit, and the freeze drying chamber. An organic solvent cold trap is fixed between the vacuum pump and the conventional cold trap, an auto-supplying device for liquid nitrogen is fixed between the organic solvent cold trap and the freeze drying chamber, which is connected respectively with the atomization tubes for cleaning in the organic solvent cold trap and the freeze drying chamber. The utility model has the advantage that the liquid nitrogen-aided refrigeration freeze-dryer not only condenses the organic solvent effectively to protect the vacuum system effectively, but also controls the freeing process of the sample well, decreases overall temperature in freeze drying chamber,thereby avoiding the ''hard surface film'' caused by the high concentration of freeze drying agent.
Description
Technical field
The utility model relates to a kind of liquid nitrogen auxiliary refrigeration and freeze dryer, can be used for the freeze-drying of medicine, belongs to refrigeration freeze dryer technical field.
Background technology
Freezing dry process is complicated heat transfer, mass transport process, and freeze-drying process and freezing process are closely related, and the latter has determined the time of freeze-drying process and the quality of dried frozen aquatic products to a certain extent.Yet in existing medicine freeze-drier, the freezing process of medicine is finished mostly on the shelf, and the rate of temperature fall of shelf is relatively slow, is generally less than 5k/min.The liquid state preparation with shelf in temperature-fall period, ice crystal forms prior to container bottom, and thermograde is relatively large in the upper heat and lower cold, preparation, it is slow that speed is pushed ahead at the ice interface, solute migration time abundance in the solution, solution surface frozen crust solute gathers more, and high concentration " top layer duricrust " phenomenon occurs easily, form one deck fine and close " duricrust " behind the high concentration superficial drying, can hinder the effusion of water vapour in the freeze-drying process, prolong freeze-drying time, increase the difficulty of dried frozen aquatic products rehydration.In the actual production process, the solute Distribution inequality that the shelf slow freezing forms also can cause the difference of residual moisture content after the medicine preparation drying, and this solute and moisture problem of uneven distribution thereof can be brought adverse influence to the storage-stable of freeze-drying process and product.So, in solution class sample shelf pre-freeze process, how to control the speed of growth of ice crystal, reduce the migration from bottom to top of sample interior solute, raising freeze-drying sample quality, energy efficient are all had great importance.In addition, the use of a large amount of organic solvents of biochemical drug production process, cause the organic solvent of drug residue under vacuum state, to enter vacuum system, and conventional cold-trap (60 ℃) can't capture these organic solvents, in a single day organic solvent enters the oil sealing rotary-vane vaccum pump, pumping fluid and potted component are with destroyed, and vacuum system can't be worked normally.
Summary of the invention
The purpose of this utility model is that a kind of organic solvent that makes of invention condenses, and vacuum system is effectively protected, and also can make the freezing process of sample controlled, prevents the liquid nitrogen auxiliary refrigeration and freeze dryer of the appearance of preparation high concentration " top layer duricrust " phenomenon.
For realizing above purpose, the technical solution of the utility model provides a kind of liquid nitrogen auxiliary refrigeration and freeze dryer, comprise vavuum pump, mechanical refrigeration unit, conventional cold-trap, cryodesiccation chamber, conventional cold-trap connects vavuum pump, mechanical refrigeration unit and cryodesiccation chamber respectively, it is characterized in that, between vavuum pump and conventional cold-trap, be provided with the organic solvent cold-trap, be provided with the liquid nitrogen automatic supplier between organic solvent cold-trap and cryodesiccation chamber, the liquid nitrogen automatic supplier is connected with cleaning mist pipe in the cryodesiccation chamber with the organic solvent cold-trap respectively.
Described liquid nitrogen automatic supplier comprises liquid nitrogen container, the low temperature seal ring, the liquid nitrogen conveyance conduit, low-temperature solenoid valve, needle-valve, electricity node Pressure gauge, safety valve, heater, temperature probe, two low-temperature solenoid valves link to each other with the cleaning mist pipe with the organic solvent cold-trap respectively, the liquid nitrogen conveyance conduit is fixed in the liquid nitrogen container by the low temperature seal ring, the terminal of liquid nitrogen conveyance conduit connects low-temperature solenoid valve, needle-valve is located at the middle part of liquid nitrogen carrier pipe, safety valve is located on the liquid nitrogen carrier pipe in needle-valve the place ahead, be positioned at the liquid nitrogen container outside, electricity node Pressure gauge is located on the liquid nitrogen carrier pipe between safety valve and the needle-valve, heater is positioned at the top of liquid nitrogen carrier pipe, and temperature probe is positioned on the heater.
The top of described liquid nitrogen conveyance conduit is far from liquid nitrogen container bottom 1cm-3cm distance.
Described heater is positioned at the top of liquid nitrogen carrier pipe, from liquid nitrogen container bottom 8cm-15cm distance.
The utility model is set up liquid nitrogen automatic supplier and organic solvent cold-trap in conventional freeze dryer.Liquid nitrogen automatic supplier one tunnel connects the cleaning mist pipe in conventional freeze dryer cryodesiccation chamber, and one the tunnel connects condenser coil in the organic solvent cold-trap.The liquid nitrogen automatic supplier is mainly finished liquid nitrogen cleans mist pipe and organic solvent cold-trap in cryodesiccation chamber conveying, after liquid nitrogen enters cryodesiccation chamber, the vaporization heat absorption, reduce the bulk temperature in the cryodesiccation chamber, the pre-freeze process of freeze-drying indoor sample can be controlled preferably, and lyophilized formulations high concentration " top layer duricrust " problem is promptly solved; After liquid nitrogen entered organic solvent cold-trap condenser coil, the vaporization heat absorption caused the interior condenser coil surface of this cold-trap to be reduced to below-120 ℃, and organic solvent can condense under this temperature mostly, thereby reaches the purpose that organic solvent captures.
It is to solve the effective way of above-mentioned two problems with the liquid nitrogen auxiliary cooling system that the utility model adopts freeze dryer.-196 ℃ approximately of liquid nitrogen temperatures, the about 210kJ/kg of the latent heat of vaporization, and most organic solvent-120 ℃ promptly curable, liquid nitrogen assists cold-trap can guarantee that the freeze dryer vacuum system do not destroyed by organic solvent.In addition, liquid nitrogen is set in cryodesiccation chamber supplies with the atomizing refrigerating plant automatically, first the freezing by liquid nitrogen system of sample finished, because liquid nitrogen temperature is lower, vaporization rate is very fast, refrigerating capacity is stronger, the automatic supply control system of liquid nitrogen can be controlled rate of temperature fall easily, and crystallization at first occurs from the teeth outwards, and liquid nitrogen refrigerating can effectively solve the interior solute of sample with combining of shelf refrigeration and distribute irregular problem, thereby improve the quality and the storage-stable of sample greatly, and energy savings consumption.
The utility model has the advantages that the liquid nitrogen auxiliary refrigeration and freeze dryer not only can make organic solvent condense; vacuum system is effectively protected; also can make the freezing process of sample obtain good control; it is globality that the freeze-drying indoor temperature reduces, and has prevented the appearance of lyophilized formulations high concentration " top layer duricrust " phenomenon.
Description of drawings
Fig. 1 is a liquid nitrogen auxiliary refrigeration and freeze dryer system architecture schematic diagram;
Fig. 2 is a liquid nitrogen automatic supplier structural representation.
The specific embodiment
The utility model is described in further detail below in conjunction with drawings and Examples.
Embodiment
As shown in Figure 1, be liquid nitrogen auxiliary refrigeration and freeze dryer system architecture schematic diagram, described liquid nitrogen auxiliary refrigeration and freeze dryer, by vavuum pump 1, mechanical refrigeration unit 2, conventional cold-trap 3, cryodesiccation chamber 4, liquid nitrogen automatic supplier 6, organic solvent cold-trap 7 is formed, conventional cold-trap 3 connects vavuum pump 1 respectively, mechanical refrigeration unit 2 and cryodesiccation chamber 4, organic solvent cold-trap 7 is installed between vavuum pump 1 and conventional cold-trap 3, liquid nitrogen automatic supplier 6 is installed between organic solvent cold-trap 7 and cryodesiccation chamber 4, and liquid nitrogen automatic supplier 6 is connected with cleaning mist pipe 5 in the cryodesiccation chamber 4 with organic solvent cold-trap 7 respectively.
Liquid nitrogen automatic supplier 6 makes liquid nitrogen can divide two-way to flow to freeze dryer 4 as required, one tunnel pipeline through freeze dryer 4 purging systems enters cleaning mist pipe 5 atomizings in the cryodesiccation chamber 4, temperature descends in the cryodesiccation chamber 4 speed and liquid nitrogen feed flow are approximated to linear relationship, cause sample pre-freeze process to obtain good control, solved only high concentration " top layer duricrust " problem of shelf pre-freeze generation; Another road is delivered to organic solvent cold-trap 6, because liquid nitrogen temperature is lower, causes organic solvent cold-trap 6 inner coil pipe temperature can reach below-120 ℃, and organic solvent can both be solidified in this concentration mostly, thereby has protected the vacuum system of freeze dryer 4.
As shown in Figure 2, be liquid nitrogen automatic supplier structural representation, described liquid nitrogen automatic supplier 6 comprises liquid nitrogen container 8, low temperature seal ring 9, liquid nitrogen conveyance conduit 10, low-temperature solenoid valve 11, needle-valve 12, electricity node Pressure gauge 13, safety valve 14, heater 15, temperature probe 16, two low-temperature solenoid valves 11 link to each other with cleaning mist pipe 5 with organic solvent cold-trap 7 respectively, liquid nitrogen conveyance conduit 10 is fixed in the liquid nitrogen container 8 by low temperature seal ring 9, the top of liquid nitrogen conveyance conduit 10 keeps the distance of about 1cm far from the liquid nitrogen container bottom, the terminal of liquid nitrogen conveyance conduit 10 connects low-temperature solenoid valve 11, needle-valve 12 is located at the middle part of liquid nitrogen carrier pipe 10, be positioned at the liquid nitrogen container outside, safety valve 14 is located on the liquid nitrogen carrier pipe 10 in needle-valve 12 the place aheads, be positioned at the liquid nitrogen container outside, on the liquid nitrogen carrier pipe 10 that electricity node Pressure gauge 13 is located between safety valve 14 and the needle-valve 12, heater 15 is positioned at the top of liquid nitrogen carrier pipe 10, from the about 10cm in liquid nitrogen container bottom, temperature probe 16 is positioned on the heater 15.
Liquid nitrogen is carried by liquid nitrogen carrier pipe 10, transmitting power comes from the rising of liquid nitrogen container 8 internal pressures, the rising of the pressure in the liquid nitrogen container 8 is derived from the heating of heater 15, heater 15 heating, liquid nitrogen is vaporized in liquid nitrogen container 8, cause liquid nitrogen container 8 internal pressures to rise, heater 15 work stop and start are by electric node Pressure gauge 13 controls, when liquid nitrogen container 8 internal pressures are low, the 13 electric node conductings of electricity node Pressure gauge, heater 15 work are when liquid nitrogen container 8 internal pressures reach setting value, the electricity node disconnects, and heater 15 quits work.The safeguard protection of container inner pressure is guaranteed safety by safety valve 14, and when liquid nitrogen container 8 internal pressures played warning value, safety valve 14 was opened, and the nitrogen of vaporization is run out of, and liquid nitrogen container 8 internal pressures reduce; When liquid nitrogen container 8 internal pressures in normal range (NR), safety valve 14 cuts out; The time length that how much is kept by low-temperature solenoid valve 11 openings of liquid nitrogen output determines that low-temperature solenoid valve 11 is opened, and liquid nitrogen is sent outside, otherwise, carry end.11 opening times of low-temperature solenoid valve are long more, and conveying capacity is big more, and the speed that liquid nitrogen is carried is regulated by needle-valve 12, and needle-valve 12 open degree are big more, and the liquid nitrogen transporting velocity is fast more; Temperature probe 16 carries out the low liquid level monitoring of liquid nitrogen, and when being lower than these temperature probe 16 present positions along with the liquid nitrogen liquid level, temperature probe 16 is measured temperature and can be raise, and when being higher than setting value, will carry out the ultralow warning of liquid level.
Described organic solvent cold-trap 7 structures and conventional cold-trap structure proximate, the condenser coil external surface area is about 1/10 of the interior condenser coil external surface area of conventional cold-trap in the organic solvent cold-trap 7, condenser coil one termination liquid nitrogen automatic supplier in the organic solvent cold-trap, a termination atmosphere.
Claims (4)
1. liquid nitrogen auxiliary refrigeration and freeze dryer, comprise vavuum pump (1), mechanical refrigeration unit (2), conventional cold-trap (3), cryodesiccation chamber (4), conventional cold-trap (3) connects vavuum pump (1) respectively, mechanical refrigeration unit (2), and cryodesiccation chamber (4), it is characterized in that, between vavuum pump (1) and conventional cold-trap (3), be provided with organic solvent cold-trap (7), be provided with liquid nitrogen automatic supplier (6) between organic solvent cold-trap (7) and cryodesiccation chamber (4), liquid nitrogen automatic supplier (6) is connected with cleaning mist pipe (5) in organic solvent cold-trap (7) and the cryodesiccation chamber (4) respectively.
2. liquid nitrogen auxiliary refrigeration and freeze dryer according to claim 1, it is characterized in that, described liquid nitrogen automatic supplier (6) comprises liquid nitrogen container (8), low temperature seal ring (9), liquid nitrogen conveyance conduit (10), low-temperature solenoid valve (11), needle-valve (12), electricity node Pressure gauge (13), safety valve (14), heater (15), temperature probe (16), two low-temperature solenoid valves (11) link to each other with cleaning mist pipe (5) with organic solvent cold-trap (7) respectively, liquid nitrogen conveyance conduit (10) is fixed in the liquid nitrogen container (8) by low temperature seal ring (9), the terminal of liquid nitrogen conveyance conduit (10) connects low-temperature solenoid valve (11), needle-valve (12) is located at the middle part of liquid nitrogen carrier pipe (10), safety valve (14) is located on the liquid nitrogen carrier pipe (10) in needle-valve (12) the place ahead, be positioned at the liquid nitrogen container outside, electricity node Pressure gauge (13) is located on the liquid nitrogen carrier pipe (10) between safety valve (14) and the needle-valve (12), heater (15) is positioned at the top of liquid nitrogen carrier pipe (10), and temperature probe (16) is positioned on the heater (15).
3. liquid nitrogen auxiliary refrigeration and freeze dryer according to claim 2 is characterized in that, the top of described liquid nitrogen conveyance conduit (10) is far from liquid nitrogen container (8) bottom 1cm-3cm distance.
4. liquid nitrogen auxiliary refrigeration and freeze dryer according to claim 2 is characterized in that, described heater (15) is positioned at the top of liquid nitrogen carrier pipe (10), from liquid nitrogen container bottom 8cm-15cm distance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520046351 CN2888373Y (en) | 2005-11-08 | 2005-11-08 | Freezing-drying machine with liquid nitrogen to assist refrigerate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520046351 CN2888373Y (en) | 2005-11-08 | 2005-11-08 | Freezing-drying machine with liquid nitrogen to assist refrigerate |
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| Publication Number | Publication Date |
|---|---|
| CN2888373Y true CN2888373Y (en) | 2007-04-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200520046351 Expired - Lifetime CN2888373Y (en) | 2005-11-08 | 2005-11-08 | Freezing-drying machine with liquid nitrogen to assist refrigerate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104785311A (en) * | 2015-03-09 | 2015-07-22 | 韩山师范学院 | Experimental type liquid nitrogen quick freezing simple device |
| CN105509393A (en) * | 2014-09-26 | 2016-04-20 | 宋占涛 | Solvent catcher taking liquid nitrogen as cold source |
| TWI612218B (en) * | 2015-07-13 | 2018-01-21 | 愛發科低溫泵股份有限公司 | Cryotrap |
| CN109442878A (en) * | 2018-11-26 | 2019-03-08 | 山东农业大学 | Multifunctional vacuum freeze drier and its application method |
| CN110095575A (en) * | 2019-05-08 | 2019-08-06 | 中国科学技术大学 | The enriching and purifying equipment of pure gas in mixed gas |
| CN114225463A (en) * | 2020-09-09 | 2022-03-25 | 阿里巴巴集团控股有限公司 | Liquid nitrogen cold trap, method for cold trapping clear liquid nitrogen, dilution refrigerator and quantum computer |
-
2005
- 2005-11-08 CN CN 200520046351 patent/CN2888373Y/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105509393A (en) * | 2014-09-26 | 2016-04-20 | 宋占涛 | Solvent catcher taking liquid nitrogen as cold source |
| CN104785311A (en) * | 2015-03-09 | 2015-07-22 | 韩山师范学院 | Experimental type liquid nitrogen quick freezing simple device |
| TWI612218B (en) * | 2015-07-13 | 2018-01-21 | 愛發科低溫泵股份有限公司 | Cryotrap |
| CN109442878A (en) * | 2018-11-26 | 2019-03-08 | 山东农业大学 | Multifunctional vacuum freeze drier and its application method |
| CN110095575A (en) * | 2019-05-08 | 2019-08-06 | 中国科学技术大学 | The enriching and purifying equipment of pure gas in mixed gas |
| CN114225463A (en) * | 2020-09-09 | 2022-03-25 | 阿里巴巴集团控股有限公司 | Liquid nitrogen cold trap, method for cold trapping clear liquid nitrogen, dilution refrigerator and quantum computer |
| CN114225463B (en) * | 2020-09-09 | 2023-03-21 | 阿里巴巴集团控股有限公司 | Liquid nitrogen cold trap, method for cold trapping clear liquid nitrogen, dilution refrigerator and quantum computer |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: SHANGHAI FULONG TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: DONGFULONG SCI-TECH CO., LTD., SHANGHAI Effective date: 20080718 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20080718 Address after: Shanghai city Minhang District Fanghe Road No. 2199, zip code: 201109 Patentee after: Shanghai Tofflon Science and Technology Co., Ltd. Address before: Shanghai city Minhang District Fanghe Road No. 2199, zip code: 201109 Patentee before: Dongfulong Science & Technology Co., Ltd., Shanghai |
|
| CX01 | Expiry of patent term |
Granted publication date: 20070411 |
|
| EXPY | Termination of patent right or utility model |