Freeze drying apparatus and method employing vapor flow monitoring and/or vacuum pressure control

• US 6,122,836 A
• Filed: 05/07/1998
• Issued: 09/26/2000
• Est. Priority Date: 05/07/1998
• Status: Expired due to Term

• Current Assignee: SP Industries Incorporated (ATS Corp.)
• Original Assignee: SP Industries Incorporated (ATS Corp.)
• Inventors: Bart, Siegfried G. Jr., Tenedini, Kenneth J.
• Primary Examiner(s): Ferensic, Denise L.
• Assistant Examiner(s): RAGONESE, ANDREA M
• Application Number:
  US09/074,248
• Time in Patent Office: 873 Days
• Field of Search: 34/192, 34/284, 34/287, 34/292, 34/293, 34/297, 34/407, 34/558, 34/559, 34/565, 34/566, 34/567, 34/570, 34/571, 34/92, 34/286, 34/237, 34/5, 73/118, 73/861.78, 73/861.33, 73/861.77, 62/126, 62/129, 62/150
• US Class Current: 34/92
• CPC Class Codes: F26B 5/06 the process involving freezing

Abstract

Freeze drying apparatus and associated lyophilization procedures are provided employing vapor flow detection and/or vacuum control for monitoring and control of the lyophilization process. The vapor flow detector, such as a windmill sensor, is disposed to monitor vapor flow from product undergoing lyophilization. In a batch process, vapor flow is collectively monitored with the vapor flow detector between the process chamber and condenser chamber, while in a manifold configuration separate vapor flow detectors are employed at each flask attachment port. A windmill sensor provides visual feedback to an operator and/or electronic feedback to a system controller. A vacuum control system is also provided for use with or independent of vapor flow detection. This vacuum control disconnects the vacuum source from the process chamber when pressure within the process chamber falls below a first predefined set point. The vacuum source is then reconnected if process chamber pressure rises above a second predefined set point.

Claims

1. A freeze drying apparatus comprising:

a process chamber for accommodating a plurality of product containers;

a condenser chamber in communication with said process chamber via a channel;

a vacuum source for producing a vacuum on said condenser chamber and process chamber; and

a vapor flow detector disposed to monitor vapor flow to said condenser chamber from product exposed in said process chamber.

2. The freeze drying apparatus of claim 1, wherein said vapor flow detector comprises a windmill sensor disposed within said channel coupling said process chamber and said condenser chamber, wherein vapor flow through said channel causes rotation of said windmill sensor.

3. The freeze drying apparatus of claim 2, wherein said windmill sensor is disposed within said channel to be visually perceptible by an operator during freeze drying processing using said freeze drying apparatus.

4. The freeze drying apparatus of claim 3, wherein said process chamber comprises a batch process chamber containing at least one shelf for holding said plurality of product containers.

5. The freeze drying apparatus of claim 1, wherein said process chamber comprises a manifold having a plurality of flask attachment ports for receiving a plurality of product containing drying flasks.

6. The freeze drying apparatus of claim 5, wherein said freeze drying apparatus further comprises at least one separate vapor flow detector associated with at least one flask attachment port for monitoring vapor flow from product within at least one drying flask connected to said at least one flask attachment port.

7. The freeze drying apparatus of claim 1, wherein said vapor flow detector comprises means for detecting a rate of drying and end of drying of product exposed in said process chamber.

8. The freeze drying apparatus of claim 7, wherein said vapor flow detector comprises means for providing visual feedback of said rate of drying and said end of drying to an operator.

9. The freeze drying apparatus of claim 7, wherein said freeze drying apparatus further comprises a process controller, and means for communicating said rate of drying and said end of drying monitored by said vapor flow detector to said process controller.

10. The freeze drying apparatus of claim 9, wherein said process controller comprises means for employing said rate of drying to automatically regulate at least one adjustable parameter of said process chamber.

11. The freeze drying apparatus of claim 1, wherein said channel comprises a secondary channel, and said freeze drying apparatus further comprises a main vapor flow channel interconnecting said process chamber and said condenser chamber, said main vapor flow channel having a larger internal diameter than said secondary channel, and wherein said freeze drying apparatus further comprises means for using said vapor flow detector to detect termination of freeze drying processing by selectively diverting vapor flow through only said secondary channel.

12. The freeze drying apparatus of claim 11, wherein said means for using comprises a first isolation valve in said main vapor flow channel and a second isolation valve in said secondary channel, and wherein said freeze drying apparatus further comprises automated means for closing said first isolation valve and opening said second isolation valve for selective sensing of vapor flow through said secondary channel using said vapor flow detector.

13. The freeze drying apparatus of claim 1, wherein said process chamber comprises a manifold having a plurality of flask attachment ports, and wherein said freeze drying apparatus further comprises means for selectively applying heat to one or more flasks coupled to said plurality of flask attachment ports.

14. The freeze drying apparatus of claim 13, wherein said condenser chamber includes a condenser cooled by a heat producing compressor, and wherein said means for selectively applying heat comprises adjustable vents for directing heat produced by said heat producing compressor onto said one or more flasks coupled to said plurality of flask attachment ports of said manifold.

15. The freeze drying apparatus of claim 1, further comprising automated control means for disconnecting said vacuum source from said condenser chamber and process chamber during freeze drying processing of product exposed in said process chamber, said automated control means initiating said disconnecting whenever vacuum pressure within said process chamber drops below a predefined set point during freeze drying processing.

16. The freeze drying apparatus of claim 15, wherein said vacuum source comprises a vacuum pump, and wherein said automated control means for disconnecting said vacuum pump comprises means for automatically shutting off said vacuum pump whenever pressure within said process chamber drops below said predefined set point during freeze drying processing of product exposed in said process chamber.

17. The freeze drying apparatus of claim 16, wherein said automated control means further comprises means for turning on said vacuum pump whenever pressure within said condenser chamber rises above a predefined upper set point during freeze drying processing of product exposed to said process chamber.

18. The freeze drying apparatus of claim 15, wherein said automated control means for disconnecting said vacuum source comprises a solenoid valve coupled between said vacuum source and said condenser and process chambers, said solenoid valve comprising means for controllably connecting/disconnecting said vacuum source from said condenser and process chambers whenever pressure within said process chamber during freeze drying processing is outside a predefined range.

19. A freeze drying apparatus for freeze drying product adapted to be contained in a frozen state in at least one flask, said freeze drying apparatus comprising:

a manifold presenting a sealed interior chamber and at least one port adapted to receive said at least one flask to place the interior of said flask and product therein in gaseous communication with said interior chamber;

a condenser associated with said interior chamber of said manifold for condensing condensible vapors present in said interior chamber;

a vacuum pump for producing a vacuum within said interior chamber of said manifold for reducing ambient pressure in said interior chamber; and

a vapor flow detector for monitoring vapor flow from product in at least one flask coupled to said manifold during freeze drying processing using said freeze drying apparatus.

20. The freeze drying apparatus of claim 19, wherein said condenser is disposed within a condenser chamber, and said manifold couples to said condenser chamber via a channel, and wherein said vapor flow detector comprises a main vapor flow detector disposed in said channel interconnecting said manifold and said condenser chamber.

21. The freeze drying apparatus of claim 20, wherein said condenser is driven by a refrigeration source, and wherein said freeze drying apparatus further includes adjustable vents between said refrigeration source and said at least one flask for selectively directing exhaust heat from said refrigeration source onto said at least one flask during freeze drying processing.

22. The freeze drying apparatus of claim 20, further comprising at least one vapor flow port detector, each vapor flow port detector being associated with one port of said manifold to detect vapor flow from product in one flask coupled to said one port.

23. The freeze drying apparatus of claim 19, wherein said vapor flow detector is associated with one port of said manifold for monitoring vapor flow from product contained within one flask coupled to said one port.

24. A freeze drying apparatus for freeze drying product, said freeze drying apparatus comprising:

a process chamber for accommodating a plurality of product containers;

a vacuum pump for producing a vacuum on said process chamber; and

a process controller connected to said vacuum pump, said process controller monitoring freeze drying within said freeze drying apparatus and during freeze drying processing selectively disconnecting said vacuum pump from said process chamber without impairing freeze drying processing within said freeze drying apparatus.

25. The freeze drying apparatus of claim 24, wherein said process controller comprises means for shutting off said vacuum pump whenever pressure within said process chamber is less than a first predefined vacuum level and for turning on said vacuum pump whenever pressure within said process chamber exceeds a second predefined vacuum level.

26. The freeze drying apparatus of claim 25, wherein said first predefined vacuum level and said second predefined vacuum level are an identical set point.

27. The freeze drying apparatus of claim 24, wherein said process controller comprises means for regulating pressure within said process chamber utilizing water vapor from said product undergoing freeze drying processing.

28. The freeze drying apparatus of claim 24, further comprising a solenoid valve coupled between said vacuum pump and said process chamber, said solenoid valve being employed by said process controller to selectively disconnect/connect said vacuum pump without impairing freeze drying processing.

29. The freeze drying apparatus of claim 28, wherein said process controller comprises means for disconnecting said vacuum pump during secondary drying of product undergoing freeze drying processing whenever pressure within said process chamber drops below a predefined vacuum level.

30. The freeze drying apparatus of claim 24, wherein said process chamber includes at least one shelf for holding said plurality of product containers, and wherein said freeze drying apparatus further comprises a condenser chamber in communication with said process chamber and a vapor flow detector disposed between said process chamber and said condenser chamber, said vapor flow detector monitoring vapor flow to said condenser chamber from product exposed in said process chamber.

31. The freeze drying apparatus of claim 24, wherein said process chamber comprises a manifold presenting a sealed interior chamber and at least one port adapted to receive at least one flask to place the interior of said flask, and product contained therein, in gaseous communication with said interior chamber, and wherein said freeze drying apparatus further comprises at least one vapor flow port detector disposed at said at least one port for monitoring vapor flow from product within at least one flask coupled thereto.

32. The freeze drying apparatus of claim 31, further comprising a condenser chamber in communication with said manifold and a main vapor flow detector disposed between said interior chamber of said manifold and said condenser chamber, said main vapor flow detector monitoring vapor flow from product in gaseous communication with said interior chamber.