Microwave-assisted separations using volatiles

• US 5,884,417 A
• Filed: 09/11/1997
• Issued: 03/23/1999
• Est. Priority Date: 02/10/1992
• Status: Expired due to Term

• Current Assignee: Her Majesty The Queen In Right of Canada As Represented By The Minister of National Defence
• Original Assignee: Her Majesty The Queen In Right of Canada As Represented By The Minister of National Defence
• Inventors: Pare, J. R. Jocelyn
• Primary Examiner(s): Gennett, Henry A.
• Assistant Examiner(s): Gravini, Steve
• Application Number:
  US08/927,581
• Time in Patent Office: 558 Days
• Field of Search: 34/259, 34/263, 34/265, 34/74, 34/76, 34/78, 34/79, 34/82, 34/92, 203/39, 203/40, 219/680, 219/686, 426/241, 426/340
• US Class Current: 34/263
• CPC Class Codes: B01D 1/0017 Use of electrical or wave energy B01D1/0029 takes precedence
• CPC Class Codes: B01D 19/0078 by vibration
• CPC Class Codes: B01J 19/126 Microwaves
• CPC Class Codes: B01J 3/008 Processes carried out under supercritical conditions
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/146 using membranes
• CPC Class Codes: G01N 30/06 Preparation

Abstract

The generation of volatiles from liquid or solid materials is enhanced and accelerated by exposure to microwave radiation. Normally the energy transfer is effected preferentially toward the liquid or solid materials over the generated gaseous volatiles. Sufficient energy is provided at a selected rate that enhances the generation of volatiles to effect removal as vapor or to produce a pressurized vapor phase. Flow-through separations from a matrix having a microwave-absorbing liquid component are conducted by exposing to microwave radiation to vaporize this component and processing the vapor either by flowing through a selective permeable membrane, or by enclosing the vapor and matrix in a confined space and flowing matrix through a selected separation medium, and recovering residual matrix. These separations are particularly useful in analysis contexts.

Claims

1. In a method for the microwave extraction of at least one natural product from a biological material, said method consisting in:

placing said biological material in an enclosure without any solvent,

making said biological material present in said enclosure undergo microwave irradiation in order to prompt the evaporation of at least a part of the water contained in said biological material, so as to enable the release of at least a part of said natural product,

separating the residual biological material from the extracted natural product,

the improvement wherein said method includes the steps of

cyclically intermittently applying reduced pressure within said enclosure during said step for the application of microwaves,

heating said enclosure during at least the essential part of said step for the application of microwaves, the combination of said steps for the application of the microwaves, the application of reduced pressure within the enclosure and the heating of the enclosure permitting the volatilization of said natural product from said biological material.

2. Method according to claim 1, characterized in that said method includes the step of subjecting the interior of said enclosure to microwave radiation/pressure cycles.

3. Method according to one of the claim 1, characterized in that said step for the separation of the residual biological material from the extract consists in:

condensing the vapour containing extracted natural product,

collecting the condensed material mixture resulting from such condensation, and

separating natural product.

4. Method according to claim 1, characterized in that at least a part of the condensed product is recycled and wherein the method includes the step of steam distillation to obtain a natural product.

5. Method according to claim 1, characterized in that said heating step is conducted at a temperature lower than 100°

C.

6. Method according to claim 1, characterized in that the microwaves used during said step of microwave irradiation have a frequency at least equal to 300 MHz.

7. Method according to claim 1, characterized in that said step of microwave irradiation is conducted so as to apply power ranging from about 100 Watts to about 65,000 Watts per Kg of product.

8. Method according to claim 1, which includes the step of imparting motion to said biological material in said enclosure.

9. A method according to claim 1, including the step of condensing separated volatilized components from a gas phase to a lower energy phase.

11. An installation suitable for the implementation of a method according to claim 1, characterized in that the installation includes

an enclosure provided with means to generate microwaves within said enclosure and having a thermostat-controlled double wall;

heating means enabling the temperature of said thermostat-controlled double wall to be regulated;

means enabling the pressure inside said enclosure to be reduced;

means to recover the extract after microwave treatment.

12. An installation according to claim 11, characterized in that said installation includes means for enabling the pressure within the enclosure to be reduced cyclically.

13. An installation according to claim 11, characterized in that it includes means for recycling of residual material.

14. An installation according to claim 11, wherein said installation includes means for condensing volatilized components.

15. An installation according to claim 11, said installation including means for effecting mechanical motion of biological material within said enclosure.

10. A method of microwave extraction of at least a natural product from a biological material containing volatilizable components, comprising

providing a matrix of biological material having volatilizable components dispersed therein,

treating said matrix with microwave energy to effect volatilization of at least one of the volatilizable components from the biological material,

cyclically intermittently applying reduced pressure during the microwave treatment, and

separating at least one volatilized component to obtain at least one natural product from the biological material.