CN101713607B - Method for producing powder through decompression, atomization, freezing and drying and device - Google Patents
Method for producing powder through decompression, atomization, freezing and drying and device Download PDFInfo
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- CN101713607B CN101713607B CN2009102630885A CN200910263088A CN101713607B CN 101713607 B CN101713607 B CN 101713607B CN 2009102630885 A CN2009102630885 A CN 2009102630885A CN 200910263088 A CN200910263088 A CN 200910263088A CN 101713607 B CN101713607 B CN 101713607B
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Abstract
The invention discloses a method for producing powder through decompression, atomization, freezing and drying and a using device. In a drying method, suspension liquid to be dried is atomized into fog drops of micro grade through an atomizer, the fog drops are fast frozen to form an ice powder when meeting low-temperature cold air in the vessel, a valve of an air inlet and outlet of the vessel is closed after the ice powder is manufactured, vacuum pumping is carried out until the pressure in the vessel achieves a set pressure at the same time, the ice powder in the vessel is in treatments such as decompression, dehydration and drying, moisture in the ice powder is gradually decreased after water vapor generated by the dehydration of the ice powder in the vessel is continuously extracted within a certain time so as to achieve the requirement of water content needed for drying a product, and a whole decompression and drying process is finished. The decompression, sublimation, the dehydration and the drying are finished in the same vessel so as to satisfy the requirements of continuous dehydration and drying. The device has the advantages of simple operation, continuous running and the like, can guarantee the quality of the product, also can directly obtain the dried powder product, and greatly shorten the drying time compared with the traditional vacuum freezing drying or normal pressure atomization freezing drying at the same time.
Description
Technical field
The present invention relates to a kind of method and apparatus of dry powder process, particularly a kind of handle contains solvent or the method for suspension convection drying powder process and the device of use of solid.
Background technology
At present, the main method that adopts is directly to utilize liquid nitrogen or liquid CO 2, utilize the ultralow temperature of above-mentioned two kinds of cryogens to obtain low temperature ice powder in the technical field of spray chilling powder process.But when directly utilizing liquid nitrogen or liquid CO 2, it is constant that the temperature of gas is difficult to, and simultaneously because can't circulating and recovering, makes the wasting of resources of above-mentioned two kinds of fluids, increased the cost of applying unit greatly.The ice powder of making must be finished in vacuum freeze dryer again, and vacuum freeze drying drying time is long, energy consumption is high, and dry products needs to pulverize, and powder is irregular.
Application number is that the application of 200720067866.X has related to a kind of vacuum freeze drier, comprise freeze drying box, heater, draining valve, water vapour coagulator, vavuum pump, inferior isolating valve, vent valve, condenser pipe, main isolating valve and dividing plate, goods to be dried are first by pre-freeze, then by distillation and the drying of finishing goods from low temperature to high temperature under the certain vacuum degree on dividing plate.But, because the ice of pre-freeze can only remove solvent in the goods by vacuum, must make that the whole dry run time is long, the energy consumption height, and also goods could obtain powder product after being must pulverize after dry, and product form is extremely irregular.
Application number is that 03278110.5 application has related to a kind of convection type vacuum freezing drying device that is used for removing the porous material solvent, form by cryogenic media jar and freeze drying chamber, contain cryogenic media in the cryogenic media jar, on freeze drying chamber, be provided with chamber cap, on freeze drying chamber, also be provided with vacuum pumping opening, vacuum pumping opening is connected in vacuum extractor, is provided with the dry gas air inlet pipe on freeze drying chamber, and freeze drying chamber is located in the cryogenic media jar.But this device does not make the goods fluidization of pre-freeze, just air-flow flows through from the pre-freeze product surface, and therefore, the effect of wearing that the convection current conduction forms is unsatisfactory, and dehumidifying in advance of the gas that enters household freezer, certainly will increase the load of freeze drying itself.
Application number is that 200420081901.X has related to the rotary freeze drying plant of a kind of shelf, comprise magnetic driver, frame, liquid nitrogen container, heater, freeze drying box, input pipe, efferent duct, condenser, vavuum pump, hydraulicefficiency elevation structure, control circuit, be provided with hydraulicefficiency elevation structure in the magnetic driver, place the Rotary cloumn in the freeze drying box to be provided with shelf, be provided with the structure of heater and liquid nitrogen spout in the freeze drying box all around.Though this device utilizes liquid nitrogen can accelerate the precooling of goods,, the essence of its drying still is to adopt the mode of vacuum freeze drying, so, can't avoid the weakness of this kind freeze drying mode.
Application number is 200820159643.0 to have related to and adopt low temperature dehumidification gas to carry out the device of atomizing freeze drying, comprise compositions such as casing, fluid bed, sack cleaner, but, the ice powder that spray chilling is made still carries out freeze drying under normal pressure, because the difference between the moisture content between moisture content in the gas and low temperature ice powder is very little, has caused whole dry run still very long, above 10 hours, utilize ultralow temperature to remove humid gas for a long time, cause the energy consumption of unit product higher.
To sum up, it is long to utilize the spray chilling combination drying to obtain dried powder ubiquity dry run at present, and energy consumption height, product need to pulverize the shortcoming of equipment complexity again.
Summary of the invention
In order to solve the shortcoming that dry products need be pulverized again and drying time is long, energy consumption is high that prior art exists, the invention provides a kind of method of atomizing freeze drying powder process and device of use of reducing pressure, utilize the low dew point gas of low temperature directly liquid to be dried to be made ice powder drying under reduced pressure again, shortened drying time, saved the energy, and the finished product that obtains is a dried powder.
Technical scheme of the present invention is: a kind of method of the atomizing freeze drying powder process of reducing pressure, and step is:
The first step, liquid to be dried atomizer through being positioned at the casing top is sprayed into casing, the liquid-drop diameter of ejection is 31～300 microns, utilize temperature in the casing be-50 ℃～-40 ℃, dew point be-60 ℃～-50 ℃ gas with the drop that enters freezing be to ice powder;
Second step, after treating that liquid freezing is the ice powder, close intake valve, then box house is vacuumized, vacuum is 0.001MPa～0.01MPa in the control casing, and gas is at-25 ℃～-10 ℃ in the control chuck, and drying is 3～5 hours then, in the chuck gas temperature rise to 10～40 ℃ dry 1～2 hour again, it is 15～250 microns powder-product that the ice pruinescence is dried to particle diameter.Gas in the chuck of casing can feed the gas in the casing in the casing chuck before vacuumizing, and can save operating cost like this.
The device that uses in the method for described decompression atomizing freeze drying powder process, described device mainly is made up of casing, chuck, atomizer, vavuum pump, casing is provided with chuck outward, the top of casing is provided with atomizer, also be provided with gas feed and gas vent on the casing, gas vent is connected with vavuum pump.Described vavuum pump is water-ring vacuum pump or rotary-vane vaccum pump, when adopting rotary-vane vaccum pump, is provided with water vapor condenser between casing and vavuum pump.The device that uses in the method for described decompression atomizing freeze drying powder process, described gas vent is connected with chuck by an arm.Gas in the container can be fed in the chuck and use, so just can save operating cost.In gas feed, be provided with just effect, middle effect and High-Performance Gas Filter.This system just can satisfy the few bacterium or the aseptic requirement of medicine, food and biogenetic products etc. fully like this
The device that uses in the method for described decompression atomizing freeze drying powder process is provided with separator in the described casing, is used for the freezing gentle flow point of ice powder is opened, and makes this ice powder rest in the casing simultaneously and finishes until drying.
The liquid-drop diameter of liquid to be dried atomizer ejection through being positioned at sealable container top is the 31-300 micron, feed temperature in the container and be low to moderate-50 ℃～-40 ℃, dew point is-60 ℃～-50 ℃ a gas, make above-mentioned two to contact, make droplet be frozen into the ice powder rapidly, after finishing the preparation of ice powder, the cryogenic gas of container is fed in the chuck of container, the gas inlet and outlet that airtight said vesse is original, the valve of openable container and vavuum pump, start vavuum pump, controlling opening of valve makes the interior pressure of container reduce to the pressure of setting, 0.001MPa-0.01MPa, solvent in the ice powder in the container is distilled at this moment, finishes until the lyophilization dehydration, and it is 15-250 micron powder-product that the ice pruinescence is dried to particle diameter.。
The preparation of the low dew point gas of low temperature can application reference number is 2008200328707 patents described " devices that prepare low dew point low temperature drying gas continuously ", the pre-cold-peace runner of main employing removes airborne moisture, adopts two-stage deep cooling cooling device to obtain the dry gas of the low dew point of continuous low temperature then.The atomising device of atomizing ice making powder also can application reference number is 200820159643.0 patents described " using the low dew point air-atomizing freeze drying fuel pulverizing plants of low temperature "
Beneficial effect:
1, need not in the whole process of the present invention to utilize liquid nitrogen or dry ice or temperature to be low to moderate-60 ℃ gas, at the gas of-50 ℃～-40 ℃ the low dew point of low temperature liquid to be dried is made the ice powder as long as adopt gas temperature, greatly reduce production cost, saved the energy.
2, the present invention is owing to directly made the ice powder to feed liquid to be dried by atomising device, and the distillation of finishing the ice powder under decompression or vacuum condition dehydrates process, there are not phenomenons such as reunion between ice powder that fluid bed causes and local inhomogeneous drying, so the particle comparison rule of the finished product dry powder that obtains.
3, the present invention has adopted the principle of vacuum dehydration drying, because the surface area of the ice powder of making is very big, compare with original vacuum freeze drying or normal pressure spray-freezing drying, the decompression atomizing freeze drying can shorten drying time greatly, can shorten to present 4～5 hours by original more than 10 hour.
4, whole dry run of the present invention reaches in the container of band low temperature chuck and finishes under lower temperature, thereby the characteristic of having guaranteed material itself process that is not dried changes, therefore, the quality for medicine, food and biogenetic products etc. keeps and needs dry product particularly suitable.
5, the used vavuum pump of the present invention is water-ring vacuum pump or rotary-vane vaccum pump, when adopting rotary-vane vaccum pump, has increased a water vapor condenser between casing and vavuum pump, has improved dewatering efficiency.
6, preparation method who the present invention relates to and device have simple and reliable for structure, and cost of equipment maintenance is low, the characteristics of economical rationality.
Description of drawings
Fig. 1 is a device schematic diagram of the present invention.
The specific embodiment
Below in conjunction with Fig. 1 the present invention is elaborated:
A kind of method of the atomizing freeze drying powder process of reducing pressure, step is:
The first step, liquid to be dried atomizer through being positioned at the casing top is sprayed into casing, liquid-drop diameter by the ejection of twin fluid atomization device or ultrasonic ultrasonic delay line memory is 31～300 microns, utilize temperature in the casing be-50 ℃～-40 ℃, dew point be-60 ℃～-50 ℃ gas with the drop that enters freezing be to ice powder;
Second step, after treating that liquid freezing is the ice powder, close intake valve, then box house is vacuumized, vacuum is 0.001MPa～0.01MPa in the control casing, and gas is at-25 ℃～-10 ℃ in the control chuck, and drying is 3～5 hours then, in the chuck gas temperature rise to 10～40 ℃ dry 1～2 hour again, it is 15～250 microns powder-product that the ice pruinescence is dried to particle diameter.Gas in the chuck of container can feed the gas in the container in the container chuck before vacuumizing, and can save operating cost like this.
This decompression atomizing freeze drying fuel pulverizing plant mainly is made up of casing 6, chuck, atomizer 7, vavuum pump 14, the casing 6 outer chucks that are provided with, the top of casing 6 is provided with atomizer 7, also is provided with gas feed and gas vent on the casing 6, and gas vent is connected with vavuum pump 14.Be provided with separator in the described casing 6, be used for the freezing gentle flow point of ice powder is opened, make this ice powder rest in the casing simultaneously and finish until drying.Described gas vent is connected with chuck by an arm.Gas in the casing 6 can be fed in the chuck and use, save operating cost.Described vavuum pump is water-ring vacuum pump or rotary-vane vaccum pump, when adopting rotary-vane vaccum pump, is provided with water vapor condenser between casing 6 and vavuum pump 14.In gas feed, be provided with just effect, middle effect and High-Performance Gas Filter, can satisfy the aseptic requirement in fields such as medicine, food like this.Described atomizer is ultrasonic ultrasonic delay line memory or twin fluid atomization device.
Concrete operating procedure is as follows: liquid material to be dried is atomized into micron-sized fine mist by twin fluid atomization device or ultrasonic ultrasonic delay line memory 7, atomizer 7 is arranged at the top of cabinets cavity, micron-sized droplet is low to moderate-50 ℃ by temperature on every side, dew point is that-60 ℃～-50 ℃ gas is cooled to the ice powder rapidly, fall on the inwall or bottom wall of casing 6, after treating that all materials are made into to ice powder, close the terminal valve of original cold air, and cold air is introduced in the chuck of this container, guarantee the cooling of wall of a container face, can not make the ice powder of container melt, valve that is connected with vavuum pump on the while openable container and startup vavuum pump, ice powder in the container enters distillation and dehydrates the stage, adjust valve opening, make the vacuum in the container reach corresponding setting value, for example, 0.01MPa, at this moment, solvent in the ice powder is distilled continuously, when remaining unchanged after the setting vacuum up in the container, enter gas at normal temperature in the container chuck, make the powder in the container continue dry until the intensification drying stage, according to material characteristic, last baking temperature can be made as 10-40 ℃ with gas temperature in the chuck, time was generally 1 hour, just can get the powder-product of drying to the end.If be provided with roughing efficiency air filter, middle effect and High-Performance Gas Filter in gas feed, this system can satisfy the few bacterium or the aseptic requirement of medicine, food and biogenetic products etc. fully.
Embodiment 1
Dry ginkgo biloba p.e prepares powder-product: get ginkgo biloba p.e 200g, add the cyclodextrine of 50g, the distilled water that adds 750g, being configured to solid content is the ginkgo biloba p.e suspension 1000g of 25%wt, make suspension atomization become the droplet of 31-300 micron with ultrasonic ultrasonic delay line memory at the container of strap clamp cover, it is-45 ℃ with temperature simultaneously, dew point is-50 ℃ low temperature and low humidity gas contact, be cooled to ice extract powder rapidly, pulverizing process is finished behind the 45min, enters the decompression lyophilization stage.At this moment, low temperature and low humidity gas in the container is fed in the chuck, temperature in the control chuck is at-20 ℃, close the terminal valve that provides and get rid of gas originally for container simultaneously, open the valve that connects vavuum pump, start vavuum pump, adjust valve opening and make that the vacuum in the container is 0.01MPa, move 4 hours continuously after, the vacuum up in the container is to 0.007MPa, refrigerating gas in the chuck is maintained 10 ℃, and operation 60min, again gas heating to 30 in the chuck ℃, operation 30min, finish whole dry run, take out dried extract powder, after measured: the particle diameter of powder is the 15-132 micron, residual water content is 5.2%wt, original identical of flavones content fundamental sum.
Embodiment 2
A kind of method for preparing milk powder with the spray chilling combination drying, is solid content the 300g milk powder adding 500g distilled water of 95%wt, be configured to the milk liquid of solid content 35.6%wt, be atomized into tiny droplet with the twin fluid atomization device, atomizing is 0.35MPa with compressed-air actuated pressure, in-50 ℃ cryogenic gas, be frozen into to ice milk powder, finish the ice making powder behind the 38min.The gas inlet and outlet valve of closing containers is opened vavuum pump and is connected valve subsequently, and starts vavuum pump, the vacuum of adjusting in the container is 0.0075MPa, the interior temperature of chuck this moment adopts-15 ℃ cryogenic gas, operation 200min, and it is dry to begin subsequently to heat up, elder generation feeds chuck to 10 ℃ air, make the powder in the container continue drying under reduced pressure 60min, dry 45min under 40 ℃ of environment finishes whole process then, the moisture of the milk powder that obtains is 4.5%wt, and particle diameter is the 20-165 micron.
Claims (8)
1. method of atomizing freeze drying powder process that reduces pressure is characterized in that step is:
The first step, liquid to be dried atomizer through being positioned at the casing top is sprayed into casing, the liquid-drop diameter of ejection is 31～300 microns, utilize temperature in the casing be-50 ℃～-40 ℃, dew point be-60 ℃～-50 ℃ gas with the drop that enters freezing be to ice powder;
Second step, after treating that liquid freezing is the ice powder, close intake valve, then box house is vacuumized, vacuum is 0.001MPa～0.01MPa in the control casing, and gas is at-25 ℃～-10 ℃ in the control chuck, and drying is 3～5 hours then, in the chuck gas temperature rise to 10～40 ℃ dry 1～2 hour again, it is 15～250 microns powder-product that the ice pruinescence is dried to particle diameter.
2. the method for a kind of atomizing freeze drying powder process of reducing pressure as claimed in claim 1 is characterized in that, in second step, the gas utilization in the chuck of casing be the gas in the container before vacuumizing.
3. the device that uses in the method for decompression atomizing freeze drying as claimed in claim 1 powder process, it is characterized in that, described device mainly is made up of casing (6), chuck, atomizer (7), vavuum pump (14), the outer chuck that is provided with of casing (6), the top of casing (6) is provided with atomizer (7), casing also is provided with gas feed and gas vent on (6), and gas vent is connected with vavuum pump (14).
4. the device that uses in the method for decompression atomizing freeze drying as claimed in claim 3 powder process is characterized in that, described casing is provided with separator in (6).
5. the device that uses in the method for decompression atomizing freeze drying as claimed in claim 3 powder process is characterized in that, described gas vent is connected with chuck by an arm.
6. the device that uses in the method for decompression atomizing freeze drying as claimed in claim 3 powder process, it is characterized in that, described vavuum pump is water-ring vacuum pump or rotary-vane vaccum pump, when adopting rotary-vane vaccum pump, is provided with water vapor condenser between casing (6) and vavuum pump (14).
7. the device that uses in the method for decompression atomizing freeze drying as claimed in claim 3 powder process is characterized in that, is provided with just effect, middle effect and High-Performance Gas Filter in gas feed.
8. the device that uses in the method for decompression atomizing freeze drying as claimed in claim 3 powder process is characterized in that, described atomizer is ultrasonic ultrasonic delay line memory or twin fluid atomization device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102630885A CN101713607B (en) | 2009-12-16 | 2009-12-16 | Method for producing powder through decompression, atomization, freezing and drying and device |
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| CN2009102630885A CN101713607B (en) | 2009-12-16 | 2009-12-16 | Method for producing powder through decompression, atomization, freezing and drying and device |
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| CN101713607A CN101713607A (en) | 2010-05-26 |
| CN101713607B true CN101713607B (en) | 2011-03-16 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2649045T3 (en) * | 2010-08-04 | 2018-01-09 | Ima Life North America Inc. | Bulk freeze-drying by spray freezing and agitated drying |
| US9945611B2 (en) | 2010-08-04 | 2018-04-17 | Ima Life North America Inc. | Bulk freeze drying using spray freezing and agitated drying |
| CN106268503B (en) * | 2015-06-29 | 2020-01-17 | 南京邮电大学 | Liquid nitrogen spray freezing granulation vacuum drying device and working method |
| CN106705574A (en) * | 2015-11-17 | 2017-05-24 | 上海东富龙科技股份有限公司 | Solid preparation fabrication equipment and method |
| CN112197514B (en) * | 2020-10-26 | 2022-02-01 | 湖南精诚制药机械有限公司 | Vacuum drying oven that likepowder medicament is dry with drying efficiency height |
| CN114192067A (en) * | 2021-12-08 | 2022-03-18 | 南通东概念新材料有限公司 | Method for preparing granules by spray drying, liquid nitrogen quick freezing and vacuum freeze drying |
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