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Supersonic freeze drying method and apparatus

A freeze dryer and ultrasonic technology, which is used in the drying of solid materials, lighting and heating equipment, and drying solid materials without heating, can solve the problems of prolonged drying time, large difference in evaporation speed, and increased cost, and can promote heat. The effect of conversion, shortening of freeze-drying time, and reduction of heat transfer resistance

Inactive Publication Date: 2010-11-03
PHARM TECH TIANJIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process takes a long time and consumes a lot of energy. Especially when freeze-drying trays, the thickness of the material layer varies greatly, and the evaporation rate varies greatly, resulting in prolonged drying time. Finally, the freeze-dried powder is agglomerated, and the effect is poor when it is re-dissolved. It needs to be pulverized. Reconstituted and re-lyophilized
At the same time, the tray-type freeze-drying process needs to process a large number of trays, including tray scraping, transportation, cleaning, etc., which requires a large workshop space and directly brings about cost increases

Method used

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  • Supersonic freeze drying method and apparatus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Red ginseng water reflux extraction, the first time 5 times the amount of water, 1 hour; the second time 3 times the amount of water, 0.5 hours; the third time 3 times the amount of water, 0.5 hours; combine the extracts, let cool, dilute hydrochloric acid to adjust the pH 2, filter, polyamide on the supernatant, rinse with water, the effluent is colorless; elute with dilute alkaline solution, collect the eluate, adjust the pH to 5 with dilute hydrochloric acid, apply macroporous resin on the acid solution, rinse with water, and use 95% ethanol For elution, collect the alcohol eluate, concentrate under reduced pressure to a solid content of 10-30% (weight), and set aside. Add an appropriate amount of mannitol and transfer to an ultrasonic freeze dryer. Under continuous ultrasound, the frequency is 15kHz, and the material is frozen; cryogenically cooled to a temperature of -40°C, kept for 4 hours, turned on a vacuum of 0.3mbar, started the condenser, and performed a temp...

Embodiment 2

[0030] Astragalus is extracted three times with water, add 5, 4, and 4 times the amount of water, each time for 1 hour, let it cool, concentrate the reverse osmosis membrane to a relative density of 1.06 (with the density of water at 20°C as a reference), and concentrate under reduced pressure to a relative density of 1.06. Density 1.1-1.15, add 95% ethanol to make alcohol concentration to 70% (volume ratio), let stand for 12 hours, filter, supernatant is concentrated to relative density 1.15-1.20, add 95% ethanol to make alcohol concentration to 85%, static Set aside for 24 hours, filter, concentrate the supernatant to a relative density of 1.2-1.25, add 8 times the amount of water for ultrasound, place it below 15°C for 24 hours, filter, concentrate the supernatant under reduced pressure to a relative density of 1.10-1.15, add an appropriate amount of mannitol , into an ultrasonic freeze dryer. Under continuous ultrasound, the frequency is 5kHz, and the material is frozen; c...

Embodiment 3

[0032]Sanqi plus 75% ethanol reflux extraction 3 times, the first time 5 times the amount of water, 1 hour; the second time 4 times the amount of water, 0.5 hours; the third time 4 times the amount of water, 0.5 hours; combined extracts, reduced pressure Concentrate without alcohol smell, apply macroporous adsorption resin, wash with water, elute with 75% ethanol, collect the eluate, and set aside; apply 941 decolorizing resin to the eluate, collect the effluent, and concentrate under reduced pressure to powder. Dissolve the powder with an appropriate amount of ethanol, slowly drop it into the aqueous solution of hydroxypropyl β-cyclodextrin under ultrasound, concentrate under reduced pressure to a relative density of 1.10-1.15, and introduce the drug solution into an ultrasonic freeze dryer. Under continuous ultrasound, the frequency is 10-15kHz, and the material is frozen; cryogenically cooled to a temperature of -50°C, kept for 4 hours, turned on a vacuum of 3mbar, started t...

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Abstract

The utility model discloses an ultrasonic freeze drying process, relating to the technical field of the freeze drying agent, mainly comprising that after the materials are dissolved in a suitable solvent, the material can be handled with the continuous ultrasonic assistance; under the vacuum freezing condition, the solvent are deeply frozen into solid state; the heat energy is continuously supplied, making the solvent in the materials sublimed into vapor state directly from the solid state; the drying process is completed after the vapor is pumped out by the vacuum system. The equipment of the utility model comprises a closed vessel, a cooling and heating system, a vacuum system, an ultrasonic device, and the relating heat insulation and sealing device. The ultrasonic freeze drying process is characterized in rapid drying speed, high production efficiency, and small labor intensity. The process and the equipment can be applied to the drying fields of the medicine, food, chemistry and other respects.

Description

technical field [0001] The invention relates to the technical field of freeze-drying, in particular to a process and equipment for completing freeze-drying under ultrasonic vibration. Background technique [0002] Substances exist in three forms: solid, liquid and gas. Under certain vacuum and temperature conditions, substances can be directly transformed from solid to gaseous. This process is a sublimation process. Sublimation technology is used to freeze substances and their solutions, supplemented by vacuum , so that the solvent in the substance sublimates directly into a gas in a solid state under freezing, and is entrained by the vacuum system, so that the material is dried under the premise of maintaining the stability of the material. The material after freeze-drying treatment has better stability, prolonged storage period, and good solubility when dissolved again. Freeze-drying technology is widely used in biological products, pharmaceuticals and food industries, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): F26B5/02F26B5/06
Inventor 孙小兵张文生
Owner PHARM TECH TIANJIN
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