CONTROLLED NUCLEATION DURING FREEZING STEP OF FREEZE DRYING CYCLE USING PRESSURE DIFFERENTIAL WATER VAPOR CO2 ICE CRYSTALS

• US 20150040420A1
• Filed: 08/06/2013
• Published: 02/12/2015
• Est. Priority Date: 08/06/2013
• Status: Active Grant

• Current Assignee: Millrock Technology, Inc.
• Original Assignee: Millrock Technology, Inc.
• Inventors: Ling, Weijia
• Granted Patent: US 9,470,453 B2
• Time in Patent Office: Days
• US Class Current: 34/298
• CPC Class Codes: F26B 5/06 the process involving freezing

Abstract

A method of controlling and enhancing the nucleation of product in a freeze dryer wherein a product is maintained at a predetermined temperature and pressure. A mixture of water vapor and CO₂ gas is introduced into a condenser chamber separate from the product chamber to create a predetermined volume of condensed frost, ice and dry ice crystals on an inner surface of the condenser chamber. The condenser chamber is connected to the product chamber and has a predetermined pressure that is greater than that of the product chamber. Upon the opening of the condenser chamber into the product chamber, gas turbulence is created that causes the condensed frost in the form of an ice fog and accompanying ice and dry ice crystals to rapidly enter the product chamber for even distribution therein to create uniform and rapid nucleation of the product in different areas of the product chamber.

Claims

1. A method of controlling and enhancing the nucleation of product in a freeze dryer, comprising:

maintaining the product at a predetermined temperature and pressure in a chamber of the freeze dryer;

introducing a mixture of water vapor and CO₂ gas into a condenser chamber separate from the product chamber to create a predetermined volume of condensed frost, ice and dry ice crystals on an inner surface of the condenser chamber, the condenser chamber being connected to the product chamber by a vapor port and having a predetermined pressure that is greater than that of the product chamber; and

opening the vapor port into the product chamber to create gas turbulence that causes the condensed frost in the form of an ice fog and accompanying ice and dry ice crystals to rapidly enter the product chamber for even distribution therein to create uniform and rapid nucleation of the product in different areas of the product chamber.

2. The method of claim 1, wherein CO₂ gas is introduced into the condenser chamber prior to the introduction of the water vapor and CO₂ gas mixture to create a dry ice layer of predetermined thickness on the inner surface of the condenser chamber to facilitate the formation of the condensed frost, ice and dry ice crystals thereon and their removal when the vapor port is opened.

3. The method of claim 1, wherein the pressure within the product chamber is about 50 Torr and the pressure within the condenser chamber is about 760 Torr when the vapor port is opened into the product chamber.

4. The method of claim 3, wherein the temperature of the product chamber is about −

5 °

C. and the temperature of the condenser chamber is about −

60°

C. to −

85°

C. when the vapor port is opened into the product chamber.

5. The method of claim 1, wherein upon contact with warmer objects during travel of the ice and dry ice crystals from the condenser chamber to the product chamber, some of the dry ice will melt and vaporize to absorb heat and generate cold gas flow to reduce the loss of the ice crystals by keeping the ice frozen and increasing the rate of travel of the ice crystals into the product chamber.

6. The method of claim 1, wherein the amount of CO₂ gas introduced into the condenser chamber should be less than the pH level of product in solution in the product chamber.