CN100455963C - Method for fast freezing liquid material used for freezing drying technique - Google Patents
Method for fast freezing liquid material used for freezing drying technique Download PDFInfo
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- CN100455963C CN100455963C CNB2006100463437A CN200610046343A CN100455963C CN 100455963 C CN100455963 C CN 100455963C CN B2006100463437 A CNB2006100463437 A CN B2006100463437A CN 200610046343 A CN200610046343 A CN 200610046343A CN 100455963 C CN100455963 C CN 100455963C
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Abstract
A quickly freezing method of liquid state materiel for froze dry technology. The freezing dry machine of it relates to freezing hothouse, cold trap and vacuum pump. Disperse frozen materiel into solvent to form liquid state materiel; start freezing dry machine to reduce the temperature of cold trap to under the freezing point of solvent. Put frozen liquid state materiel into container on the inside shelf of the freezing hothouse and start vacuum pump; vacuumize the freezing hothouse and cold trap to vaporize large solvent of frozen liquid state materiel. Then the temperature reduced and the ebullition started with the condition of low press and low temperature and it froze into solid quickly and completely. The character of it is quick, low consumption of energy, high speed of sublimation and dryness, simple process, high efficiency and able to be industrialized.
Description
Technical field:
The present invention relates to a kind of method of quick freezing liquid material of Freeze Drying Technique.
Background technology:
At present in fields such as the production and processing of products such as food, medicine, biological products and chemical reagent and superfine powder, nano powder preparation, when needs freeze liquid material, generally the technology of Cai Yonging is that frozen material is placed in the low temperature environment, by frozen object and low temperature environment heat-shift, directly make frozen material be cooled to the following temperature of freezing point gradually, thereby reach the purpose of freezing.Concrete refrigerating process has: one, direct freezing, the direct freezing of liquid material is, the integral container of a certain amount of liquid material of splendid attire is placed in the low temperature environment, in the freeze drier as precooling in advance, in the cold airflow or low temperature refrigerator medium, making material and environment heat-shift and slowly lowering the temperature freezing is solid until freeze all; Two, spray chilling method, the spray chilling method of liquid material are to use special-purpose sprayer that liquid material is atomized becomes the drop of small scale, and drop falls into low-temperature refrigerant liquid (as liquid nitrogen) under the drive of blowing gas; Drop is frozen into solid after entering cold-producing medium rapidly.The defective that exists is: it is slow that direct freezing is freezed speed, and energy consumption is big; When a large amount of material integral body carry out direct when freezing, scars freeze fully real after, there is temperature difference greatly on its inner and surface, the scars surface temperature is low, and the scars surface area is little, causes lyophilization speed subsequently low; The spray chilling complex process need to consume a large amount of cold-producing mediums, and production efficiency is low, is difficult to realize industrialization.
Summary of the invention:
The object of the present invention is to provide a kind of fast, low energy consumption, lyophilization speed height, technology is simple, efficient is high and can realize the industrialized method that is used for the quick freezing liquid material of Freeze Drying Technique.
Enforcement of the present invention needs a particular device: freeze drier.This freeze drier comprises freeze drying chamber, cold-trap, vavuum pump.The indoor shelf that is provided with of freeze drying is placed a container on the shelf, freeze drying chamber is connected with cold-trap through valve by pipeline.Be provided with condenser in the cold-trap, low-temperature refrigerant or refrigerant liquid are housed in the condenser, this condenser is connected with refrigeration compressor.Cold-trap is connected with vavuum pump through valve by pipeline.
The method step of the said quick freezing liquid material of the present invention is:
1, will be frozen raw material and be distributed in the solvent, form liquid material;
2, start freeze drier, condenser temperature is reduced to below the freezing point of solvent;
3, the liquid material that is frozen is contained in the container on the indoor shelf of freeze drying;
4, start vavuum pump,, make a large amount of evaporations of the solvent that is frozen in the liquid material and temperature reduces and boiling under low pressure, the cryogenic conditions takes place, promptly freeze to be solid then fully for freeze drying chamber and cold-trap vacuumize.
General experiment at present can both reach the requirement of the technology of the present invention with freeze drier, freeze-drying of food machine and pharmaceutical purpose freeze drier.The function of vavuum pump is to provide the vacuum necessary degree for freeze drying chamber and cold-trap, and in time discharges the permanent gas that vacuum chamber bleeds and emits.Do not require that vavuum pump can discharge the steam that solvent evaporation produces in a large number.The purpose of building vacuum environment for vacuum chamber and cold-trap is, reduces environmental pressure, and the liquid material boiling point is reduced, impel solvent rapidly evaporation cause the liquid material boiling; Reduce the gas flow resistance, the promotion solvent vapour migrates to cold-trap by freeze drying chamber and the device that is condensed captures.Condenser is arranged in the cold-trap, be connected with low-temperature refrigerant or refrigerant fluid in the condenser pipe, the condenser hull-skin temperature must be reduced to below the solvent freezing point temperature.Condenser to have adapt with the material total amount that requires to freeze, enough big capture areas, thereby make cold-trap have the ability of enough big capture solvent vapour.
It is liquid material that the material that is frozen among the present invention requires, and solid material need be dispersed in the flowable object that forms solution or colloid or emulsion or suspension in the solvent or wherein comprise relatively large volatizable material.Its solvent of the liquid material that is frozen can be inorganic solvents such as water, ammoniacal liquor, also can be cyclohexane, the tert-butyl alcohol, acetate, organic solvents such as benzene.The high volatility of solvent, the latent heat of vaporization is big, and freezing point and normal temperature are near helping realizing that vacuum evaporation freezes; The content that is frozen solvent in the object can not be too low, otherwise may not exclusively freeze reality.Prepare nano-powder technology for freeze-drying, solvent is few in the freezing object, remains in the quantity of solvent deficiency in the scars after can causing vacuum evaporation to be freezed, and causes final prepared powder granule skewness, reunites between the particle.
Be frozen object in container during splendid attire, its volume and surface area will be in suitable proportions, and surface area is crossed conference and taken bigger shelf area, causes waste and reduces production efficiency; Surface area is too little may to be caused from the time that is evacuated down to boiling and prolongs slightly, or the exhaust capacity of vavuum pump and the outlet capacity of catching of cold-trap are required height.The container of splendid attire liquid material can be the container that materials such as canister, glass container, ceramic vessel and organic polymer or composite are made.
The present invention compares the advantage that possesses with background technology: being frozen material can freeze in the very short time, and energy consumption is low.Material scars internal and external temperature unanimity, surface configuration is rough and uneven in surface, is the loose structure that there are a large amount of perforation holes inside, and bigger distillation interface is arranged, and will improve lyophilization speed greatly.Compare with spray chilling, technology simply is convenient to operation, does not need to consume cold-producing medium, and the production efficiency height is suitable for suitability for industrialized production.
Description of drawings:
Fig. 1 is a structural representation of the present utility model.
Parts label in the accompanying drawing is: 1 is freeze drier, and 2 is shelf, and 3 is container, and 4 is valve, and 5 is that cold-trap, 6 is that condenser, 7 is that valve, 8 is vavuum pump.
The specific embodiment:
The required particular device of enforcement of the present invention is a freeze drier.This freeze drier comprises freeze drying chamber, cold-trap, vavuum pump.The indoor shelf that is provided with of freeze drying is placed a container on the shelf, freeze drying chamber is connected with cold-trap through valve by pipeline.Be provided with condenser in the cold-trap, low-temperature refrigerant or refrigerant liquid are housed in the condenser, this condenser is connected with refrigeration compressor.Cold-trap is connected with vavuum pump through valve by pipeline.
Embodiment 1: the vacuum evaporation of the aluminum subacetate aqueous solution in certain model freeze drier is freezing
1, the aluminum subacetate solid with 1mo1 is added to the water, and stirs to be prepared into the 2000mL aluminum subacetate aqueous solution;
2, open cold lyophilizer makes condenser temperature be reduced to below-40 ℃ (automatic control system of this model freeze drier is set, and only-40 ℃ the time, could open vavuum pump when condenser temperature is lower than);
3, the aluminum subacetate aqueous solution directly being put into surface area is about 500cm
2The stainless steel square plate in, square plate is placed on the indoor shelf of freeze drying;
4, start vavuum pump, for freeze drying box and cold-trap vacuumize.After about 5 minutes, the pressure drop in the vacuum chamber is low to moderate 200Pa, and aluminum subacetate solution comes to life.Continue to vacuumize, begin to occur ice crystal in the solution suddenly, freeze all is the entity of loose structure-20 ℃, that the surface is rough and uneven in surface, there are a large amount of perforation holes inside in less than one minute time then.
Embodiment 2: the vacuum evaporation of the aqueous solution of Kiwi berry magma in certain model freeze drier is freezing
1, will make Kiwi berry magma with juice extractor after the fresh Kiwi berry peeling, in the glass beaker of 200mL, add 50mL Kiwi berry magma and 50mL water and stir into uniform liquid material;
2, start freeze drier, make condenser temperature be reduced to below-40 ℃ (automatic control system of this model freeze drier is set, and only-40 ℃ the time, could open vavuum pump when condenser temperature is lower than);
3, beaker is placed on the shelf in the freeze drier, closes the freeze drying chamber door;
4, start vavuum pump, for freeze drying chamber and cold-trap vacuumize.After about 7 minutes, the pressure drop in the vacuum chamber is low to moderate below the 200Pa, and Kiwi berry solution begins bubbling and seethes with excitement then.Continue to vacuumize, the boiling of solution stops, and moments later begins to occur ice crystal in the solution suddenly, and freeze all is a light green color entity-28 ℃, rough and uneven in surface, the alveolate texture in surface in less than one minute time then.
Claims (4)
1, a kind of method that is used for the quick freezing liquid material of Freeze Drying Technique, the enforcement of this method needs a particular device: freeze drier, this freeze drier comprises freeze drying chamber, cold-trap, vavuum pump; The indoor shelf that is provided with of freeze drying is placed a container on the shelf, freeze drying chamber is connected with cold-trap through valve by pipeline; Be provided with condenser in the cold-trap, low-temperature refrigerant or refrigerant liquid are housed in the condenser, this condenser is connected with refrigeration compressor; Cold-trap is connected with vavuum pump through valve by pipeline; It is characterized in that:
The method step of said quick freezing liquid material is:
(1), will be frozen raw material is distributed in the solvent formation liquid material;
(2), start freeze drier, condenser temperature is reduced to below the freezing point of solvent;
(3), the liquid material that is frozen is contained in the container on the indoor shelf of freeze drying;
(4), start vavuum pump, for freeze drying chamber and cold-trap vacuumize, make a large amount of evaporations of the solvent that is frozen in the liquid material and temperature reduces and boiling under low pressure, the cryogenic conditions takes place, promptly freeze to be solid then fully.
2, a kind of method that is used for the quick freezing liquid material of Freeze Drying Technique according to claim 1, it is characterized in that: said liquid material is the flowable object that comprises relatively large volatizable material.
3, a kind of method that is used for the quick freezing liquid material of Freeze Drying Technique according to claim 1, it is characterized in that: said solvent is water, ammoniacal liquor, cyclohexane, the tert-butyl alcohol, acetate or benzene.
4, a kind of method that is used for the quick freezing liquid material of Freeze Drying Technique according to claim 1, it is characterized in that: said container is the container that canister, glass container, ceramic vessel or high-molecular organic material are made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100463437A CN100455963C (en) | 2006-04-18 | 2006-04-18 | Method for fast freezing liquid material used for freezing drying technique |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100463437A CN100455963C (en) | 2006-04-18 | 2006-04-18 | Method for fast freezing liquid material used for freezing drying technique |
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| Publication Number | Publication Date |
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| CN1888800A CN1888800A (en) | 2007-01-03 |
| CN100455963C true CN100455963C (en) | 2009-01-28 |
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| CNB2006100463437A Expired - Fee Related CN100455963C (en) | 2006-04-18 | 2006-04-18 | Method for fast freezing liquid material used for freezing drying technique |
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| CN101231249B (en) * | 2008-02-26 | 2010-06-02 | 东北大学 | Vacuum low temperature microscopic visualizer |
| CN103968649B (en) * | 2014-05-13 | 2015-12-02 | 上海理工大学 | A kind of freeze-drying method and corollary equipment |
| CN103968647B (en) * | 2014-05-15 | 2016-06-01 | 济南康众医药科技开发有限公司 | The drying means of a kind of gold sesame |
| WO2017178740A1 (en) * | 2016-04-14 | 2017-10-19 | Jean Delaveau | Freeze-drying method and device |
| CN111773760A (en) * | 2019-04-04 | 2020-10-16 | 应急管理部化学品登记中心 | Vacuum freeze-drying type solid-liquid separation method |
| CN111773759A (en) * | 2019-04-04 | 2020-10-16 | 应急管理部化学品登记中心 | Vacuum freeze-drying type solid-liquid separation device |
| CN112656004A (en) * | 2020-12-07 | 2021-04-16 | 上饶农业技术创新研究院 | Pholiota nameko glassy state drying system |
| CN115014047A (en) * | 2022-05-30 | 2022-09-06 | 南京威尔药业科技有限公司 | Method for producing tert-butyl alcohol by using freeze dryer |
| CN116086139A (en) * | 2023-02-08 | 2023-05-09 | 天津科技大学 | Solid malt extract spray freeze drying device and method capable of reducing dimethyl sulfur content |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB932576A (en) * | 1960-04-29 | 1963-07-31 | Pillsbury Co | Drying apparatus and method |
| US3384979A (en) * | 1965-08-28 | 1968-05-28 | Centre Nat Rech Scient | System for evaporating and cooling a liquid injected in vacuo |
| JPS61234764A (en) * | 1985-04-10 | 1986-10-20 | Osaka Gas Co Ltd | Freeze-drying of liquid substance |
| CN1006327B (en) * | 1988-02-16 | 1990-01-03 | 共和真空技术株式会社 | Freeze dry process and freeze drier |
| JPH0587453A (en) * | 1991-09-25 | 1993-04-06 | Ii P Japan Kk | Heat pump type vacuum-evaporation and drying apparatus |
| CN2352909Y (en) * | 1998-08-28 | 1999-12-08 | 张祯儒 | Freezing type drying machine |
| CN2416463Y (en) * | 2000-04-11 | 2001-01-24 | 北京天利医药设备有限公司 | Vacuum freezing dryer |
| CN2651678Y (en) * | 2003-06-26 | 2004-10-27 | 上海俊乐制冷自控元件有限公司 | Multifunctional experimental refrigerating drier |
| CN2695888Y (en) * | 2004-04-29 | 2005-04-27 | 上海远东制药机械总厂 | Vacuum freezing drier |
| CN1737477A (en) * | 2004-08-17 | 2006-02-22 | 韩鸿兴 | Shelf rotary type refrigeration drying apparatus |
-
2006
- 2006-04-18 CN CNB2006100463437A patent/CN100455963C/en not_active Expired - Fee Related
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB932576A (en) * | 1960-04-29 | 1963-07-31 | Pillsbury Co | Drying apparatus and method |
| US3384979A (en) * | 1965-08-28 | 1968-05-28 | Centre Nat Rech Scient | System for evaporating and cooling a liquid injected in vacuo |
| JPS61234764A (en) * | 1985-04-10 | 1986-10-20 | Osaka Gas Co Ltd | Freeze-drying of liquid substance |
| CN1006327B (en) * | 1988-02-16 | 1990-01-03 | 共和真空技术株式会社 | Freeze dry process and freeze drier |
| JPH0587453A (en) * | 1991-09-25 | 1993-04-06 | Ii P Japan Kk | Heat pump type vacuum-evaporation and drying apparatus |
| CN2352909Y (en) * | 1998-08-28 | 1999-12-08 | 张祯儒 | Freezing type drying machine |
| CN2416463Y (en) * | 2000-04-11 | 2001-01-24 | 北京天利医药设备有限公司 | Vacuum freezing dryer |
| CN2651678Y (en) * | 2003-06-26 | 2004-10-27 | 上海俊乐制冷自控元件有限公司 | Multifunctional experimental refrigerating drier |
| CN2695888Y (en) * | 2004-04-29 | 2005-04-27 | 上海远东制药机械总厂 | Vacuum freezing drier |
| CN1737477A (en) * | 2004-08-17 | 2006-02-22 | 韩鸿兴 | Shelf rotary type refrigeration drying apparatus |
Non-Patent Citations (4)
| Title |
|---|
| ZLG-0.2型真空冷冻干燥机的研制. 徐成海，张世伟，喻漫陆，关奎之.真空与低温，第5卷第2期. 1999 |
| ZLG-0.2型真空冷冻干燥机的研制. 徐成海，张世伟，喻漫陆，关奎之.真空与低温，第5卷第2期. 1999 * |
| 真空冷冻干燥法制备纳米氧化铝陶瓷粉的实验研究. 刘军，徐成海，窦新生.真空，第41卷第4期. 2004 |
| 真空冷冻干燥法制备纳米氧化铝陶瓷粉的实验研究. 刘军，徐成海，窦新生.真空，第41卷第4期. 2004 * |
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Granted publication date: 20090128 Termination date: 20100418 |