Microwave-assisted chemical synthesis instrument with fixed tuning

• US 6,630,652 B2
• Filed: 05/03/2002
• Issued: 10/07/2003
• Est. Priority Date: 01/31/2001
• Status: Expired due to Fees

• Current Assignee: CEM Global LLC
• Original Assignee: CEM Global LLC
• Inventors: Jennings, William Edward
• Primary Examiner(s): Leung, Philip H.
• Application Number:
  US10/063,628
• Publication Number:
  US 20020117498A1
• Time in Patent Office: 522 Days
• Field of Search: 219/679, 219/686, 219/704, 219/705, 219/707, 219/710, 219/711, 219/718, 219/715, 219/716, 204/157.43, 422/21, 422/81.12, 422/81.13
• US Class Current: 219/679
• CPC Class Codes: B01J 19/126 Microwaves
• CPC Class Codes: B01J 2219/00058 Temperature measurement
• CPC Class Codes: B01J 2219/00063 of the reactants
• CPC Class Codes: B01J 2219/00065 Pressure measurement
• CPC Class Codes: B01J 2219/00094 Jackets
• CPC Class Codes: B01J 2219/002 inside the reactor
• CPC Class Codes: B01J 2219/0024 other than of the reactor or heat exchange system
• CPC Class Codes: B01J 2219/1209 Features relating to the reactor or vessel
• CPC Class Codes: B01J 2219/1233 Closure means, such as lids, caps, seals B01J3/03 takes precedence; pressure relief systems in the lid, e.g. rupture discs B01J2219/0027
• CPC Class Codes: B01J 2219/1269 Microwave guides
• CPC Class Codes: B01J 2219/1275 Controlling the microwave irradiation variables
• CPC Class Codes: H01P 7/06 Cavity resonators
• CPC Class Codes: H05B 6/806 for laboratory use

Abstract

A method is disclosed for carrying out microwave-assisted chemical reactions. The method includes the steps of adding reagents to a pressure-resistant microwave-transparent vessel, securing the vessel against pressure release with a penetrable septum made of a material that can be penetrated by a needle while surrounding and sealing against the needle even after penetration to thereby maintaining the pressure integrity of the vessel, thereafter inserting a needle through the penetrable septum and into the pressure-secured vessel to provide fluid communication to the interior of the scaled pressure-resistant vessel through the needle, applying mechanical pressure against the septum while the needle is inserted therethrough, and irradiating the vessel and its contents with microwaves with the needle inserted therein.

Claims

1. A method of carrying out microwave-assisted chemical reactions the method comprising:

adding reagents to a pressure-resistant microwave-transparent vessel;

securing the vessel against pressure release with a penetrable septum made of a material that can be penetrated by a needle while surrounding and scaling against the needle even after penetration to thereby maintain the pressure integrity of the vessel;

thereafter inserting a needle through the penetrable septum and into the pressure-secured vessel to provide fluid communication to the interior of the sealed. pressure-resistant vessel through the needle;

applying mechanical pressure against the septum while the needle is inserted therethrough; and

irradiating the vessel and its contents with microwaves with the needle inserted therein.

2. A method according to claim 1 and further comprising removing the needle from the vessel following the step of irradiating the vessel.

3. A method according to claim 2 comprising inserting the needle into a second vessel following the step of removing it from the initial vessel.

4. A method according to claim 3 comprising irradiating the second vessel with microwaves flowing the step of inserting the needle into the second vessel.

5. A method according to claim 1 comprising monitoring the temperature of vessel or its contents while irradiating the vessel and its contents with microwaves.

6. A method according claim 1 comprising monitoring the pressure inside the vessel while irradiating the vessel and its contents with microwaves.

7. A method according to claim 5 or 6 comprising moderating the application of microwaves to the vessel and its contents based upon the monitored results.

8. A method of carrying out microwave-assisted chemical reactions the method comprising:

adding reagents to a plurality of pressure-resistant microwave-transparent vessels;

securing each of the vessels against pressure release with a penetrable septum made of a material that can be penetrated by a needle while surrounding and seating against the needle even after penetration to thereby maintain the pressure integrity of the vessel;

thereafter inserting a needle through the seal of a first of the vessels and into the pressure-scoured vessel to provide fluid communication to the interior of the scaled vessel through the needle with permanently breaching the seal;

applying mechanical pressure against the septum while the needle is inserted therethrough;

irradiating the vessel and its contents with microwaves while monitoring the pressure inside and temperature of the vessel;

moderating the application of microwaves to the vessel in response to the monitored temperature and pressure;

removing the needle from the first vessel following the irradiation and moderating steps and without permanently breaching the seal of the vessel; and

repeating the inserting, irradiating, monitoring, moderating and removing steps for the second and successive vessels of the plurality of vessels.

9. A method according to claim 8 comprising adding a different set of reagents to at least the second vessel.

10. A method according to claim 8 comprising adding a different set of reagents to each vessel.

11. A method according to claim 8 wherein the step of moderating the application of microwaves comprises moderating the microwave power.

12. A method according to claim 8 wherein the step of moderating the application of microwaves comprises moderating the duty cycle.

13. A method according to claim 8 wherein the step of moderating the application of microwaves comprises physically moderating the transmission of microwaves between a microwave source and the vessel.

14. A method according to claim 8 wherein the step of monitoring the temperature comprises optically monitoring the temperature without invading the vessel.

15. A method according to claim 8 wherein the step of monitoring the pressure comprises monitoring the pressure with a transducer positioned in a sealed flow path that communicates with the interior of the vessel through the needle.