CN106468500B - Freeze drying method of energy-saving freeze drying device - Google Patents
Freeze drying method of energy-saving freeze drying deviceDownload PDFInfo
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- CN106468500B CN106468500BCN201510509594.3ACN201510509594ACN106468500BCN 106468500 BCN106468500 BCN 106468500BCN 201510509594 ACN201510509594 ACN 201510509594ACN 106468500 BCN106468500 BCN 106468500B
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Abstract
Translated fromChinese
Description
Technical Field
The invention relates to the technical field of refrigeration systems, in particular to a freeze drying method of a freeze drying device, which has the advantages of good system safety performance, quick freeze drying time and energy conservation.
Background
Vacuum freeze-drying or freeze-drying is as follows: the product is pre-frozen, and then proper sublimation heat is provided under a certain vacuum environment, so that the moisture or the solvent in the frozen product is converted into water vapor, and the aim of dehydrating the product is fulfilled. This can greatly extend the shelf life or shelf life of the product. The combination of this vacuum technique and the freezing technique is a freeze vacuum dryer.
The freeze dryer in the prior art consists of two major core systems:
one system is a vacuum drying system which provides a suitable vacuum environment, e.g. below 100Pa, for the product to be dried.
The system comprises adrying box 01, ashelf 02, afirst isolation valve 03, acondenser 04, acondensing coil 05, asecond isolation valve 06, avacuum pump 07 and the like.
The other system is a refrigeration system, which provides energy for freezing a product or condensing water vapor sublimated during drying of the product into ice by a low-temperature condensing coil of a condenser through pressure difference between a drying box and the condenser. Such as: the shelf temperature of the drying box is below minus 40 ℃, and the condensing coil of the condenser is below minus 50 ℃.
The refrigeration system is divided into a direct expansion type circulation system and a direct expansion type indirect circulation system. The direct expansion type circulating system comprises a refrigerationcompression condensing unit 08, a condenserelectromagnetic valve 09, acondenser throttle valve 010, acondensing coil 05 and the like. The direct expansion type indirect circulating system is switched and comprises a drying boxelectromagnetic valve 011, a dryingbox throttle valve 012, a shared refrigerationcompression condensing unit 08, arefrigeration heat exchanger 013 and the like. The other side of theheat exchanger 013 is a circulating system which can be cooled or heated and is composed of a circulatingpump 014, aheater 015, heat conducting oil, ashelf 02 and the like. The direct expansion type circulation system and the direct expansion type indirect circulation system share the same refrigeration compression condensing unit.
The prior art scheme has the following defects:
1) the shelves carrying the frozen and sublimated products must withstand a certain pressure (or pressure) to prevent potential risks, but if the direct expansion type circulation system and the direct expansion type indirect circulation system share the same refrigeration compression and condensation unit through switching, the shelves must instantaneously exceed the design pressure of the shelves when the heat exchangers are damaged to cause refrigerant leakage, and therefore, the shelves must use a certain amount of materials in consideration of strength.
2) Due to the fact that the consumable materials are large, the time for cooling the shelf of the drying box to the proper temperature and keeping the temperature is prolonged. If the shelf reaches-40 ℃ and continues, it takes longer due to the characteristic that some products are difficult to freeze. Power consumed by the compressor to cool down if no product is placed: 32kw · 2h equals 64kw · h. According to 1m215kg of products are placed on the loading area, the temperature reduction time of the drying box is 5h, and the consumed power reaches 32 kw.5 h which is 160 kw.h.
3) The product is cooled by placing a tray or a penicillin bottle of a surrounding frame on a shelf. Because the shelf and the tray have certain flatness errors, the tray is allowed to deform after being used for many times, and the penicillin bottles in the enclosing frame are in line contact with the shelf. Therefore, the heat transfer through the surface-to-surface conduction mode is very small, and the heat transfer is realized by the convection heat exchange mode of air and products in a large quantity. Static convective heat transfer allows for a longer time for temperature uniformity of the product on the shelf to equilibrate.
In summary, in the prior art, the same refrigeration compression condensing unit is adopted in the refrigeration system, and the direct expansion type circulation system and the direct expansion type indirect circulation system are used by switching, so that the shelf is inevitably large in material consumption and cost, the power consumption for freeze drying of the product is high, and the temperature uniformity of the product on the shelf needs a longer time to reach balance due to the adoption of static convection.
Disclosure of Invention
In view of the above-mentioned deficiencies of the prior art, the present invention aims to provide a freeze-drying method of a freeze-drying device, which has a simple structure, good operation safety, low cost and energy saving, and can greatly reduce the energy consumed by vacuum freeze-drying.
In order to solve the problems in the prior art, the adopted specific technical scheme is as follows:
an energy-saving freeze drying device comprises a vacuum pump, a condenser and a drying box; the vacuum pump is arranged on one side of the condenser, the drying box is arranged on the other side of the condenser, a first isolation valve is arranged between the condenser and the drying box, and the first isolation valve can realize communication and isolation between the condenser and the drying box; a condenser solenoid valve and a condenser throttle valve are sequentially arranged between the refrigeration compression condensing unit and the condensing coil; the drying cabinet is characterized in that a shelf is arranged in the drying cabinet, a heater, a heat exchanger and a circulating pump which are connected in sequence are arranged below the drying cabinet, and the heater and the circulating pump are connected to two sides of the shelf respectively.
And an air exhaust port end of the vacuum pump penetrates through the upper part in the condenser, and a second isolating valve is arranged between the air exhaust port of the vacuum pump and the condenser.
The invention also discloses a freeze drying method of the energy-saving freeze drying device, which comprises the following steps:
s1, pre-cooling a condenser;
s2, loading products: opening a drying box door, loading the product, and closing the drying box door after loading;
s3, pre-vacuumizing of the system: starting a vacuum pump to operate, opening an isolation valve II, and vacuumizing the condenser;
s4, vacuumizing the system; when the vacuum degree in the condenser reaches below half atmospheric pressure, the first isolation valve is opened, and the drying box is vacuumized;
s5, primary drying;
s6, secondary drying;
s7, finishing freeze-drying: closing the first isolation valve and the second isolation valve in sequence, and opening air release valves on the drying box and the condenser respectively to enable the interiors of the drying box and the condenser to recover to be at the atmospheric pressure;
s8, unloading products: opening the door of the drying box, and taking out the product;
and S9, defrosting the condenser.
In a preferred technical solution, the pre-cooling the condenser in step S1 includes: and closing the first isolation valve, starting the compression condensing unit, connecting a condenser electromagnetic valve, and supplying liquid to the condensing coil by a condenser throttle valve.
In a preferred embodiment, the primary drying step in step S5 is: when the system meets the process requirements and lasts for a period of time, starting the circulating pump, starting the heater, and heating the heat conducting oil of the system to raise the temperature; and after the system heat conducting oil is heated and reaches the set process temperature value, the set process temperature value is continued for a period of time.
In a preferred technical solution, the step of secondary drying in step S6 is: when the temperature of the product reaches above 0 ℃ and lasts for a period of time, cooling water is switched on according to the requirement of a process temperature set value, heat exchange is carried out through one side of a heat exchanger, and the cooling water is input into a shelf of a drying box through a circulating pump; when the temperature of the heat-conducting oil in the shelf is reduced to the set value of the process temperature, the heat-conducting oil is continuously kept for a period of time; when the product temperature is close to 5 ℃ different from the shelf temperature, the temperature is maintained for a period of time.
In a preferred embodiment, the process temperature set value of step S5 is set by product characteristics or data obtained by experiments.
In a preferred embodiment, the process temperature set value of step S6 is set by product characteristics or data obtained by experiments.
By adopting the technical scheme, compared with the prior art, the freeze drying method of the energy-saving freeze drying device has the technical effects that: the invention adopts the condenser which can independently refrigerate and cool and the vacuum freezing and drying system which can circularly heat or cool, and utilizes the physical phenomenon that the boiling point of water is also reduced along with the reduction of the environmental pressure, namely, the pressure of the drying system is reduced or the vacuum degree is increased, so that the product on the shelf in the drying box is evaporated and rapidly cooled when the temperature of the product is lower than the temperature of the product. The dynamic convection mode is adopted, so that the temperature uniformity of the product on the shelf is good, the energy consumption of pre-freezing of the product is greatly reduced, and the vacuum freeze drying of the product is realized.
Drawings
FIG. 1 is a schematic view showing the overall structure of a freeze-drying apparatus according to the prior art;
FIG. 2 is a schematic diagram of the overall structure of an energy-saving freeze drying device according to the present invention;
fig. 3 is a diagram of the three states of the water at different pressures and temperatures in a three-phase diagram.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific examples below. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
As shown in figure 2 of the drawings, in which,
an energy-saving freeze drying device comprises a vacuum pump 5, acondenser 6 and adrying box 3; the vacuum pump 5 is arranged on one side of thecondenser 6, thedrying box 3 is arranged on the other side of thecondenser 6, afirst isolation valve 9 is arranged between thecondenser 6 and thedrying box 3, and thefirst isolation valve 9 can realize communication and isolation between thecondenser 6 and thedrying box 3; a condensing coil 11 is arranged in thecondenser 6, a refrigerationcompression condensing unit 12 connected with the condensing coil 11 is arranged below thecondenser 6, and a condenserelectromagnetic valve 13 and acondenser throttle valve 14 are sequentially arranged between the refrigerationcompression condensing unit 12 and the condensing coil 11; a shelf 4 is arranged in thedrying box 3, a heater 16, aheat exchanger 17 and a circulatingpump 18 which are connected in sequence are arranged below thedrying box 3, and the heater 16 and the circulating pump 16 are connected to two sides of the shelf 4 respectively.
An air exhaust opening end of the vacuum pump 5 penetrates through the upper part in thecondenser 6, and asecond isolation valve 10 is arranged between the air exhaust opening of the vacuum pump 5 and thecondenser 6.
The following describes the solution of the invention in principle according to fig. 3:
the boiling point of water at 1 atmosphere is 100 ℃. The freezing point is 0 ℃. Water has a boiling point that decreases below one atmosphere. The boiling point coincides with the freezing point over time, at which the pressure of the three-phase water is 611 Pa. I.e. the water is gradually converted to ice. When the pressure in the drying aggregate had dropped below 13Pa, the temperature of the ice was already-40 ℃.
Water is converted to steam at sub-atmospheric pressures, where vaporization requires the absorption of its own heat, on average about 590 kcal/kg. The subfreezing sublimation is water vapor and needs to absorb its own heat, on average about 670 kcal/kg. Without the supply of external heat, the temperature of the water will drop.
This process must continuously provide this higher vacuum level. I.e. the pressure or vacuum in the drying box to which it corresponds must be lower than the saturated vapour pressure to which the product is frozen.
Because of the dynamic vacuum environment, the pressure uniformity in the drying box is better, water is evaporated at a certain temperature, and the evaporation speed of the surface is basically consistent.
Average self heat in the vacuum cooling process:
0.6kg/m2.hr×590kcal/kg＝354kcal/m2.hr＝0.41kw，
the resulting consumption was 0.41kw × 5hr — 2.05kw.
Such as evaporation capacity of 2.3kg/m2.hr at 20 deg.C,
its own heat: 2.3kg/m2. hr. times.590 kcal/kg. 860 ═ 1.58 kw.
The self energy is generated by the action of the vacuum pump for vacuum pumping, and the performance of the vacuum pump can reach the low-temperature requirement of the product. When the pre-vacuumizing is started, the product is not cooled until the vacuum degree reaches the corresponding saturated vapor pressure below the initial temperature of the product, and the temperature is reduced. For example, a product temperature of 20 ℃ corresponds to a saturated vapor pressure of 2340 Pa. If the product is required to reach-40 ℃, the corresponding saturated vapor pressure is 12.8 Pa.
E.g. as 1m2The freeze dryer is loaded with 15kg of pure water with a thickness of 15mm, and the heat required when the temperature is reduced to-40 ℃ is as follows:
15kg×{〔20-0〕+80+[0-(-40)]}＝2100kcal
because the vacuum pump is used for vacuumizing, the cooling time is as follows:
2100 kcal/m2.hr, 6hr, where only the average heat of vaporization (or sublimation) is considered, the actual time will be shorter.
According to 1m2Compared with the prior technical scheme, the energy consumption of the vacuum pump configured by the freeze dryer is greatly reduced by nearly 36 times, wherein the power of the vacuum pump is 0.75kw, and the energy consumption of the vacuum pump is 0.75kw multiplied by 6hr which is 4.5kw.
The invention also discloses a freeze-drying method of the energy-saving freeze-drying device, and the operation process of the technical scheme of the invention is described according to the figure 2 as follows:
1. pre-cooled condenser 6 (which can be carried out simultaneously with the loading of the product)
And closing thefirst isolation valve 9. And (5) connecting a cooling water system, and starting the refrigerationcompression condensing unit 12. Theelectromagnetic valve 13 of the condenser is slightly connected, thethrottle valve 14 of the condenser supplies liquid (refrigerant) to the condensing coil 11, and the condensing coil 11 in thecondenser 6 is cooled to be lower than minus 40 ℃.
2. Loading product
The door of the dryingoven 3 is opened, the product (tray or vial with enclosure) is loaded, and after loading, the door of the drying oven is closed.
3. System pre-evacuation
The vacuum pump 5 is started to operate. And slightly waiting, opening asecond isolation valve 10 and vacuumizing thecondenser 6.
4. System evacuation
When the vacuum in thecondenser 6 reaches half atmospheric pressure, for example, below 50KPa, thefirst isolation valve 9 is opened. Thedrying box 3 is evacuated. The whole system is in a vacuum state at the moment.
5. Primary drying process
⑴ when the system reaches a process required vacuum degree of below 10Pa, and continues for a period of time, thecirculation pump 18 is started, the heater 16 is started, and the system heat conducting oil is ready to be heated and heated.
⑵ when the system oil rises and reaches a process set point, such as 50 deg.C, and continues at a constant temperature set point for a period of time.
The set value of the process temperature in the process can be set by carrying out multi-stage heating and heat preservation time according to product characteristics or data obtained by tests.
6. Secondary drying process
⑴ when the product temperature reaches a temperature above 0 deg.C, and for a period of time.
⑵ the cooling water is switched on according to the requirement of the process temperature set value as 40 ℃, the heat exchange process is carried out through one side of theheat exchanger 17, the temperature of the heat conduction oil is reduced, and the heat is input into the shelf 4 of thedrying box 3 through the circulatingpump 18, the heat is transferred to the product through the heat conduction oil in the shelf 4, and the temperature of the product is reduced.
⑶, when the temperature of the thermal oil in the shelf 4 falls to the set value, and is maintained for a constant period of time.
⑷ when the product temperature approaches the shelf 4 temperature (by around 5 c) and for a constant period of time.
The process temperature set value in the process can be set by the product characteristics or the data obtained by the test in a multi-stage cooling and heat preservation time manner.
7. End of lyophilization
⑴ closing thefirst isolation valve 9 and thesecond isolation valve 10 in sequence;
⑵ thepurge valves 20 on thedrying box 3 and thecondenser 6 are opened respectively to restore the inside of thedrying box 3 and thecondenser 6 to an atmospheric pressure.
8. Unloading products
And opening the door of the drying box, and taking out the product.
9. Thecondenser 6 defrosts.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, and any modifications and equivalents thereof within the spirit and scope of the present invention are included therein.
Claims (3)
1. A freeze-drying method of an energy-saving freeze-drying device is characterized in that: the freeze drying device comprises a vacuum pump, a condenser and a drying box; the vacuum pump is arranged on one side of the condenser, the drying box is arranged on the other side of the condenser, a first isolation valve is arranged between the condenser and the drying box, and the first isolation valve can realize communication and isolation between the condenser and the drying box; a condenser solenoid valve and a condenser throttle valve are sequentially arranged between the refrigeration compression condensing unit and the condensing coil; a shelf is arranged in the drying box, a heater, a heat exchanger and a circulating pump which are connected in sequence are arranged below the drying box, and the heater and the circulating pump are respectively connected to two sides of the shelf; an air exhaust port end of the vacuum pump penetrates through the upper part in the condenser, and a second isolating valve is arranged between the air exhaust port of the vacuum pump and the condenser;
the freeze-drying method comprises the following steps:
s1, pre-cooling condenser: closing the isolation valve I, starting the compression condensing unit, connecting a condenser electromagnetic valve, and supplying liquid to the condensing coil by a condenser throttle valve;
s2, loading products: opening a drying box door, loading the product, and closing the drying box door after loading;
s3, pre-vacuumizing of the system: starting a vacuum pump to operate, opening an isolation valve II, and vacuumizing the condenser;
s4, vacuumizing the system; when the vacuum degree in the condenser reaches below half atmospheric pressure, the first isolation valve is opened, and the drying box is vacuumized;
s5, primary drying: when the system meets the process requirements and lasts for a period of time, starting the circulating pump, starting the heater, and heating the heat conducting oil of the system to raise the temperature; after the system heat conducting oil is heated and reaches the set value of the process temperature, the set value of the process temperature is continued for a period of time;
s6, secondary drying: when the temperature of the product reaches above 0 ℃ and lasts for a period of time, cooling water is switched on according to the requirement of a process temperature set value, heat exchange is carried out through one side of a heat exchanger, and the cooling water is input into a shelf of a drying box through a circulating pump; when the temperature of the heat-conducting oil in the shelf is reduced to the set value of the process temperature, the heat-conducting oil is continuously kept for a period of time; when the difference between the product temperature and the shelf temperature is close to 5 ℃, continuing for a period of time;
s7, finishing freeze-drying: closing the first isolation valve and the second isolation valve in sequence, and opening air release valves on the drying box and the condenser respectively to enable the interiors of the drying box and the condenser to recover to be at the atmospheric pressure;
s8, unloading products: opening the door of the drying box, and taking out the product;
and S9, defrosting the condenser.
2. The freeze-drying method of an energy-saving freeze-drying device according to claim 1, wherein the process temperature set value of step S5 is set by product characteristics or experimental data.
3. The freeze-drying method of an energy-saving freeze-drying device according to claim 1, wherein the process temperature set value of step S6 is set by product characteristics or experimental data.
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| CN107228529A (en)* | 2017-07-07 | 2017-10-03 | 河南瑞凌科技有限公司 | A kind of family expenses ex situ freeze dryer |
| CN108955099A (en)* | 2018-09-18 | 2018-12-07 | 迪茗（上海）智能科技有限公司 | A kind of freeze-drying apparatus and method |
| CN117026679A (en)* | 2022-10-08 | 2023-11-10 | 中煤（北京）印务有限公司 | Method and equipment for preventing excessive deformation of printing paper |
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| US7640756B2 (en)* | 2005-06-14 | 2010-01-05 | American Air Liquide, Inc. | Lyophilization unit with liquid nitrogen cooling |
| CN101518494A (en)* | 2009-03-23 | 2009-09-02 | 上海东富龙科技股份有限公司 | Full-automatic refrigeration control method |
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| TR01 | Transfer of patent right | Effective date of registration:20211228 Address after:No. 88, group 39, Xingang village, Wangbao Town, Qidong City, Nantong City, Jiangsu Province, 226000 Patentee after:Jiangsu Fudong freeze drying equipment Co.,Ltd. Address before:201209 No. 1066, Gugao Road, Caolu Town, Pudong New Area, Shanghai Patentee before:SHANGHAI PUDONG FREEZE DRYER EQUIPMENT Co.,Ltd. | |
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