Large-scale drying device and method capable of shortening probiotic feed liquid freeze-drying time
Technical Field
The invention belongs to the technical field of vacuum freeze drying, and particularly relates to a large-scale production drying device and method capable of effectively shortening the drying time of probiotic feed liquid, which are particularly suitable for drying heat-sensitive materials such as liquid food, medicines and the like and preparing powder particles.
Background
Spray freeze drying is the combination of spray and freeze drying technology, and the reduction of the size of atomized liquid drops is favorable for improving sublimation rate, so that the subsequent drying is more uniform, the spray freeze drying is superior to other drying technologies in the aspects of product structure, quality, volatile matters, preservation of bioactive compounds and the like, and the spray freeze drying can produce powder with good fluidity, large specific surface area and high dissolving speed. Spray freeze-drying is generally carried out by transferring the frozen particles to trays, bottles or fixed beds in a freeze-dryer after spray freezing is completed. However, the drying efficiency is low due to poor integration of the apparatus, and other technical problems such as discontinuity of the spray freeze-drying process or difficulty in process scale-up are also caused. In addition, the inconvenience of cryogenic liquid handling needs to be addressed. The invention is an integrated spray freeze drying device, the process is continuous, low-temperature liquid does not need to be processed, the drying speed can be effectively improved, and the device has important significance for the production of high value-added food, medicines and biological products.
Patent CN 108709369a proposes an ultrasonic spray freeze-drying device, which mainly comprises an ultrasonic spray device, an ultrasonic controller, a freeze-drying device, an intelligent transmission system, etc. the invention directly enters into a cold medium for freezing after spraying, but needs the transmission system to transfer ice particles into a freeze-drying machine for freeze-drying.
Patent CN 102226629a proposes a fluidized bed spray freeze drying device, which couples fluidization, cold spray coating, drying separation processes, and can make atomization, freezing, drying, and separation completed in the same equipment. However, the patent needs to be filled with refrigerants such as liquid nitrogen, dry ice and the like, and low-temperature and low-humidity gas needs to be continuously filled for cocurrent flowing, so that the load of a heat exchange system is increased.
Patent CN 201293522 proposes that a spray freeze-drying powder-making device using low-temperature low-dew-point gas consists of a box body, a fluidized bed, an atomizer and a bag-type dust remover. The device uses low-temperature low-dew-point gas to directly prepare the liquid to be dried into ice powder without using liquid nitrogen and other refrigerants. However, the device still needs to continuously introduce the drying gas for a long time, which causes higher energy consumption of unit product.
Patent CN 101713607A proposes a device for preparing powder by decompression spray freeze drying, which mainly comprises a box body, a jacket, an atomizer and a vacuum pump. However, the patent only designs the drying chamber, and the degree of integration of the equipment is low.
Therefore, how to improve the integration degree of the spray freeze drying equipment, shorten the drying time and reduce the energy consumption is a problem to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides an integrated large-scale production drying device capable of effectively shortening the drying time of probiotics, and is a spray freezing and drying device.
The invention also provides a process method capable of effectively shortening the drying time of the batch processing of the probiotic liquid.
The technical problem to be solved by the invention is realized by the following technical scheme:
the utility model provides a can effectively shorten probiotic feed liquid drying time's scale production drying device which characterized in that: the equipment mainly comprises a freezing system, a spraying system, a dust removal system, a vacuum system, a heating system and an electrical control system, wherein the freezing system comprises a circulating refrigerator, a condenser and a centrifugal fan, refrigerant liquid of the circulating refrigerator is connected to the condenser through a first branch of a refrigerant liquid pipeline, and a drying chamber is connected to the centrifugal fan through a cold air circulating pipeline; the spraying system comprises a two-fluid atomizer, a peristaltic pump and an air compressor, wherein an air inlet is formed in the side wall of the two-fluid atomizer and connected with an interface of the air compressor, and a liquid inlet is formed in the side wall of the two-fluid atomizer and used for feeding materials through the peristaltic pump; the dust removal system comprises a cyclone separator and a bag-type dust collector, wherein an inlet of the cyclone separator is connected to the drying chamber through a cold air circulation pipeline, an outlet of the cyclone separator is connected with the bag-type dust collector through a pipeline, and the bag-type dust collector is connected to the centrifugal fan through a circulation pipeline; the vacuum system comprises a drying chamber, a rotary-vane vacuum pump and a cold trap, wherein the rotary-vane vacuum pump is connected to the drying chamber through the cold trap, a second branch of the refrigerating fluid pipeline is connected to the cold trap, and the cold trap is connected to a vacuum gauge pipe arranged on a vacuum pipeline of the drying chamber; the heating system is an electric heater arranged at the bottom of the drying chamber; the electric control system comprises a programmable controller, a frequency converter, a power supply, a system control panel, a vacuum gauge and the like which are arranged in a control cabinet.
And the outside of the drying chamber, the outside of the cold trap and the outside of the condenser are all wrapped by heat-insulating materials, so that the load of the circulating refrigerator is reduced.
And a circulating cold air inlet is arranged at the center above the drying chamber.
And the two-fluid atomizer is positioned at the top of the drying chamber, atomized liquid drops and circulating cold air are in the downstream direction, so that the liquid drops can be frozen in the falling process, and are collected at the bottom of the drying chamber for freeze drying.
And a water outlet is arranged at the bottom of the cold air circulating pipeline, and the outside of the cold air circulating pipeline is wrapped by a heat-insulating material.
And the cold trap and the condenser are provided with a water outlet and a refrigerant liquid discharge port.
And, electrical control system still includes the temperature sensor who installs on cold wind circulating line to and install in the manometer of air compressor machine gas outlet.
Moreover, the drying chamber is made of stainless steel materials.
A drying method of a large-scale production drying device capable of effectively shortening the drying time of probiotic feed liquid comprises the following steps:
1) pre-cooling in a drying chamber: closing valves of a second branch pipeline of the refrigerating fluid pipeline and all water outlets, and opening a valve of a first branch pipeline of the refrigerating fluid pipeline; closing a vacuum pipeline valve, isolating a cold air circulating pipeline from the vacuum pipeline, setting the circulating refrigeration temperature to be-80 ℃, and starting a circulating refrigerator to enable the temperature of a condenser to reach about-40 ℃; opening valves of an air inlet and an air outlet of the drying chamber, and communicating the drying chamber with a dust removal system and a refrigeration system; starting a centrifugal fan, setting the air speed of cold air to be 2-5m/s, and reducing the temperature of the drying chamber to about minus 40 ℃ to minus 50 ℃;
2) material atomization: after the pre-cooling is finished, the atomizer is placed in the atomizer mounting hole to be fixed; setting atomization pressure of 0.2-0.3MPa and feeding speed of a peristaltic pump of 10-40ml/min, starting the peristaltic pump to feed, closing the peristaltic pump after feeding is finished, taking out the atomizer, and sealing a fixed port;
3) vacuumizing: opening a valve of a second branch pipeline of the refrigerating fluid pipeline to reduce the temperature of the cold trap to about minus 80 ℃; closing the valve of the first branch pipeline of the refrigerant liquid pipeline; opening a vacuum pipeline valve after the fan is closed; closing the air inlet and air outlet valves of the drying chamber, and isolating the drying chamber from the dedusting system and the freezing system; opening a vacuum pump to carry out vacuum pumping treatment on the interior of the drying chamber;
4) drying materials: setting the heating temperature to be 35-45 ℃, turning on the electric heater, recording the change of the vacuum degree in the drying process, and stopping drying when the pressure of the drying chamber is lower than 4.4 Pa;
5) and (4) finishing drying: stopping drying after the pressure of the drying chamber meets the requirement, firstly closing the circulating refrigerator, closing the electric heater, closing the vacuum pump and opening the water outlet of the vacuum pipeline; and opening the drying chamber when the pressure of the drying chamber is changed to normal pressure, taking out the materials, and finishing drying.
The invention has the advantages and beneficial effects that:
1. according to the large-scale production drying device and the drying method capable of effectively shortening the drying time of the probiotic feed liquid, a refrigerant is not needed in the whole process, the circulating refrigerator provides low-temperature gas, the atomized probiotic liquid is quickly frozen into ice powder under the action of a cold environment (cold gas and cold plate surface), the low-temperature liquid is not needed to be processed, and the cost and the energy consumption are obviously saved.
2. The large-scale production drying device and the drying method which can effectively shorten the drying time of the probiotic feed liquid directly freeze the feed liquid to be dried into micro powder after atomization in the drying chamber, and prepare the probiotic micro powder through the vacuum freeze drying process, the whole process is completed in the same equipment, the frozen micro powder does not need to be transferred, and the equipment integration degree is high.
3. The large-scale production drying device and the drying method which can effectively shorten the drying time of the probiotic feed liquid have the advantages that atomized liquid drops and circulating cold air are in the forward flow direction, the atomized liquid drops can be fully contacted with the drying cold air in the falling process, the rapid freezing is realized, the equipment has high freezing efficiency, and the single-batch processing capacity is large.
4. According to the large-scale production drying device and the drying method capable of effectively shortening the drying time of the probiotic feed liquid, the electric detection control system further comprises a temperature measuring resistor arranged in the drying chamber, the temperature of the material is detected through the temperature sensor, the heating temperature of the material is adjusted through the control cabinet, the drying temperature of the feed liquid is controlled within a reasonable range, the quality of the product is guaranteed, the device and the method are very suitable for drying heat-sensitive materials such as probiotics and food, and meanwhile, the drying time is short.
5. The large-scale production drying device and the drying method which can effectively shorten the drying time of the probiotic feed liquid adopt the principle of freeze drying, the surface area of the atomized feed liquid is very large, compared with the original vacuum freeze drying, the spray freeze drying can shorten the drying time, and the dried product has uniform particle size and regular shape.
6. According to the large-scale production drying device and the drying method capable of effectively shortening the drying time of the probiotic feed liquid, the refrigerating liquid pipeline is wrapped by the heat insulation material, the cold air circulating pipeline adopts the closed loop, the condenser is additionally arranged, the air in the cold air circulating pipeline can be kept in a low-temperature and dry state, the inner wall of the drying chamber is free of frost, the cold trap is additionally arranged between the vacuum pump and the drying chamber, and the service life of the vacuum pump is prolonged.
7. The large-scale production drying device and the drying method which can effectively shorten the drying time of the probiotic feed liquid adopt two-stage gas filtering devices of the cyclone separator and the bag-type dust remover, can effectively prevent the pollution of a cold air circulating pipeline, and are convenient to clean and maintain.
8. The large-scale production drying device and the drying method which can effectively shorten the drying time of the probiotic feed liquid have the characteristics of simple structure and high integration degree, and can be used for quickly and massively producing heat-sensitive materials such as food, probiotics and the like.
9. The invention relates to a large-scale production drying device and a drying method capable of effectively shortening the drying time of probiotic feed liquid, which adopts a spray freeze drying process to directly dry the solution and the emulsion into a powdery probiotic product without secondary crushing processing, and the obtained powder has small particle size and small particle size distribution range, and the freeze-dried powder has lower cost and less investment in storage and transportation.
10. The large-scale production drying device and the drying method can effectively shorten the drying time of the probiotic feed liquid, dry products can be directly packaged for use, and if the dry products are added into various foods, the activity of probiotics is effectively maintained, the production flow is shortened, the preparation method is simple and efficient, and the drying device and the drying method are convenient for customers to use.
11. According to the large-scale production drying device and the drying method capable of effectively shortening the drying time of the probiotic feed liquid, the processed probiotic micro powder has a porous structure and a large specific surface area, so that the whole drying process is shorter, and the survival of probiotic flora is facilitated.
12. The large-scale production drying device and the drying method for effectively shortening the drying time of the probiotic feed liquid provided by the invention atomize the probiotic feed liquid at a low temperature, the probiotic feed is quickly frozen into particles at a low temperature, a small ice crystal structure can be generated in the quick freezing process, the survival of probiotics is facilitated, and the freeze drying process is especially obvious for keeping the activity of the probiotics.
Drawings
FIG. 1 is a schematic view of the structure of a spray freeze-drying apparatus according to the present invention;
FIG. 2 is a graph comparing spray freeze-drying time and conventional freeze-drying time;
FIG. 3 is a graph showing the particle size distribution of the obtained powder product.
Description of the reference numerals
1-electric heater, 2-temperature sensor, 3-drying chamber, 4-two fluid atomizer, 5-feeding hole, 6-pressure gas inlet, 7-needle gas inlet, 8-atomization pressure regulating valve, 9-needle pressure regulating valve, 10-air compressor, 11-peristaltic pump, 12-system control panel, 13-vacuum gauge, 14-control cabinet, 15-bracket, 16-valve, 17-valve, 18-cycle refrigerator, 19-valve, 20-valve, 21-rotary-vane vacuum pump, 22-cold trap, 23-condenser, 24-temperature sensor, 25-temperature sensor, 26-refrigerant liquid discharge port, 27-refrigerant liquid discharge port, 28-condensed water outlet, 29-a condensed water outlet, 30-a centrifugal fan, 31-a condensed water outlet, 32-a cyclone separator, 33-a valve, 34-a bag-type dust remover, 35-a vacuum gauge pipe, 36-a valve, 37-a temperature sensor and 38-a valve.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
A large-scale production drying device capable of effectively shortening probiotic drying time comprises a freezing system, a spraying system, a dust removal system, a vacuum system, a heating system and an electrical control system.
The refrigerating system comprises a circulation refrigerator 18, a condenser 23 and a centrifugal fan 30. The circulating refrigerator 18 provides low-temperature liquid for the condenser 23 through a first branch of a refrigerant liquid pipeline, a temperature sensor 25 is arranged in the condenser to control the temperature of the condenser to be reduced to a preset value, a valve 16 and a valve 20 are arranged on the first branch of the refrigerant liquid pipeline, and a refrigerant liquid discharge port 27 for periodically replacing the refrigerant liquid is arranged below the condenser. When the drying chamber 3 is precooled, the atomizer is taken down and the mounting hole is sealed, and the centrifugal fan 30 makes cold air circulate in a closed loop formed by the condenser 23, the drying chamber 3, the dust removal system and the centrifugal fan 30. The outside of the cold air circulation loop is wrapped by heat insulation materials, so that the load of the circulation refrigerating machine is reduced. The air inlet pipeline is provided with a temperature sensor 37 for collecting the inlet air temperature, and the bottom of the drying chamber is provided with a temperature sensor 2 for collecting the drying chamber temperature and the material temperature. The bottom of the cold air circulation pipeline is provided with a condensed water outlet 31, the bottom of the condenser is provided with a condensed water outlet 28, and condensed water in the pipeline can be discharged in time to avoid pipeline pollution. The air inlet of the cold air circulating pipeline is provided with a valve 38, and the lower air outlet is provided with a valve 33, which is used for being isolated from the vacuum system during drying.
The spraying system comprises a two-fluid atomizer 4, a peristaltic pump 11 and an air compressor 10. The two-fluid atomizer 4 is arranged at the top of the drying chamber 3, materials are conveyed to the feed port 5 through the peristaltic pump 11, pressure gas generated by the air compressor 10 is conveyed to the pressure gas inlet 6 through a pipeline, and the atomization pressure is adjusted through the atomization pressure adjusting valve 8. In order to prevent the materials from freezing in the atomizer, a through needle is arranged in the atomizer, pressure gas enters the atomizer through a through needle gas inlet 7 to enable the through needle to act, and the magnitude of the through needle acting force is controlled by a through needle pressure regulating valve 9. The particle size of the generated liquid drops can be adjusted according to the pressure, the liquid inlet quantity and the diameter of the nozzle. The two-fluid atomizer 4 is positioned at a cold air inlet, the falling direction of atomized liquid drops is the same as the flow direction of cold air, the heat transfer rate is high, and the liquid drops can be frozen in the air and at the bottom of the drying chamber.
The dust removal system comprises a cyclone separator 32 and a bag-type dust collector 34. The inlet of the cyclone separator 32 is connected to the drying chamber 3 through a cold air circulation line, and the outlet is connected to a bag-type dust collector 34 through a line. The liquid drops suspended in the air are subjected to primary dust removal in the cyclone separator, and the bag-type dust remover is a secondary dust removal device. The bag-type dust collector 34 is connected to the centrifugal fan through a cold air circulation line.
The vacuum system comprises a drying chamber 3, a rotary vane vacuum pump 21 and a cold trap 22. The second branch of the refrigerant circuit is provided with a valve 17 and a valve 19 for regulating the flow of refrigerant, and a refrigerant discharge port 29 is arranged below the cold trap 22. The vacuum pump 21 is communicated with the cold trap and the drying chamber through pipelines to form a closed loop, the drying chamber forms negative pressure after the vacuum pump is started, and sublimed water vapor is captured through the cold trap.
The heating system comprises an electric heater 1. The electric heater 1 is positioned at the bottom end of the drying chamber, and the heating temperature is adjustable.
The electric control system is arranged in a control cabinet 14 above the bracket 15 and comprises a programmable controller, a frequency converter, a power supply, a system control panel 12 and a vacuum gauge 13. A vacuum gauge 35 is arranged on a vacuum pipeline from the cold trap to the drying chamber to collect pressure signals of the drying chamber, and a vacuum gauge 13 displays the vacuum degree of the drying chamber in real time. Temperature signals collected by the temperature sensor 2, the temperature sensor 37, the temperature sensor 25 and the temperature sensor 24 are controlled by a PLC, and a system control panel can set parameters of the spray freeze drying process.
An integrated large-scale production drying method capable of effectively shortening probiotic drying time takes probiotic liquid as an experimental material, and drying comprises the following steps:
1) pre-cooling in a drying chamber: closing the valves 17 and 19 of the second branch of the refrigerant circuit, closing the condensate outlets 28, 29, 31, and opening the valves 16 and 20 of the first branch of the refrigerant circuit; closing the vacuum pipeline valve 36, isolating the cold air circulation pipeline from the vacuum pipeline, setting the circulation refrigeration temperature of the circulation refrigerator 18 to be-80 ℃, and starting the circulation refrigerator to enable the temperature of the condenser 23 to reach about-40 ℃; opening an air inlet valve 38 and an air outlet valve 33 of the drying chamber, and communicating the drying chamber with a dust removal system and a refrigeration system; starting the centrifugal fan 30, and setting the air speed of cold air to be 4m/s to reduce the temperature of the drying chamber to about minus 45 ℃;
2) material atomization: after the pre-cooling is finished, the two-fluid atomizer 4 is placed above the drying chamber 3 and fixed in an atomizer mounting hole, and the diameter of a spray head is 1 mm; setting an atomization pressure of 0.2MPa, setting a feeding speed of 20ml/min of a peristaltic pump 11 through a system control panel 12, starting the peristaltic pump to feed, closing the peristaltic pump after feeding is finished, taking out the atomizer, and sealing a fixed port;
3) vacuumizing: opening a valve 17 and a valve 19 of a second branch pipeline of the refrigerating fluid pipeline to reduce the temperature of the cold trap 22 to about minus 80 ℃; closing valves 16 and 20 of the first branch of the refrigerant fluid circuit; after the centrifugal fan 30 is closed, the vacuum pipeline valve 36 is opened; closing the air inlet valve 38 and the air outlet valve 33 of the drying chamber, and isolating the drying chamber 3 from the dedusting system and the freezing system; opening a vacuum pump 21 to carry out vacuum pumping treatment on the inside of the drying chamber;
4) drying materials: setting the heating temperature to 35 ℃, turning on the electric heater 1, recording the change of the vacuum degree of the vacuum gauge 13 in the drying process, and stopping drying when the pressure in the drying chamber is lower than 4.4 Pa;
5) and (4) finishing drying: stopping the drying test after the pressure of the drying chamber meets the requirement, firstly closing the circulating refrigerator 18, closing the electric heater 1, closing the vacuum pump 21, and slowly opening the condensed water outlet 29 of the vacuum pipeline to release the pressure of the drying chamber; and opening the drying chamber when the pressure of the drying chamber is changed to normal pressure, taking out the materials, and finishing drying. The condensed water outlet 28 and the condensed water outlet 31 are opened.
The whole drying process of the probiotic liquid can be completed within 3-5 hours (figure 2), the water content of the dried powder product is lower than 5%, and the particle size distribution of the powder is shown in figure 3.
This spray freeze-drying integrated device accomplishes whole material atomizing, liquid drop freezing, vacuum freeze-drying process in the drying chamber, and the freezing process need not use low-temperature liquid, avoids freezing liquid and material contact, freezes the material and need not to shift directly dry in the drying chamber, avoids the contaminated risk of material completely. The probiotic liquid is atomized and quickly frozen into ice particles in a low-temperature environment, and the generated ice particles are fine, so that the activity of the probiotic is favorably maintained. The specific surface area of the probiotic liquid drops generated in the atomization process is larger, the ice sublimation speed is higher, the drying time is shorter, and the survival rate of the probiotics is higher. The closed operation of the system further improves the sterility of the spray freeze drying process, does not pollute the environment and reduces the production energy consumption and the processing cost. The probiotic micro powder obtained after drying has small particle size and small particle size distribution range, and does not need secondary crushing processing. The drying process is carried out under negative pressure, the heating temperature is controllable, and the method is also suitable for spray freeze drying of other heat-sensitive materials.
Although the embodiments of the present invention and the accompanying drawings have been disclosed for illustrative purposes, those skilled in the art will appreciate that various substitutions, alterations, and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and thus the scope of the invention is not limited to the embodiments and drawings disclosed.