IP Library Granted Patent US 8,875,981
Granted Patent B2
US 8,875,981 · App. 13/490,717 · Granted Nov 4, 2014

System and method for a microreactor

Inventors: Brian Neltner (Somerville, MA); David M. King (Canton, MA); Rick Bryan Woodruff (Boulder, CO)
Assignee: Navolta LLC
B23K1/0008B01J19/0093B01J19/0046B23K2201/36B01J2219/00795B01J2219/00822B01J2219/00835B01J2219/00869B01J2219/00873B01J2219/00876B01J2219/00842B01J2219/00286B01J2219/00495B01J2219/00511B01J2219/0052B01J2219/00585B01J2219/0059B01J2219/00747
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Quick Facts
Patent No.
US 8,875,981
App. No.
13/490,717
Granted
Nov 4, 2014
Kind
B2
Abstract

A cartridge microreactor includes a tubular heater, a metal capillary reaction tubing and a brazing alloy. The tubular heater includes an inner tube surrounded by an outer heater sheath. The metal capillary reaction tubing has a high aspect ratio, an inlet port and an outlet port and is wrapped around the tubular heater so that it is in intimate thermal contact with the heater sheath. The brazing alloy permanently bonds the tubular heater with the metal capillary reaction tubing. The metal capillary reaction tubing is configured to be heated by the tubular heater and is configured to receive one or more reactants through the inlet port and to allow the reactants to react under a selected temperature and pressure and to produce one or more products exiting through the outlet port.

Claims (46)

1. A cartridge microreactor comprising:

a tubular heater comprising an inner tube surrounded by an outer heater sheath;

a metal capillary reaction tubing comprising an inlet port and an outlet port and being wrapped around the tubular heater so that it is in intimate thermal contact with the heater sheath; and

a brazing alloy permanently bonding the tubular heater with the metal capillary reaction tubing; and

wherein the metal capillary reaction tubing is configured to be heated by the tubular heater and is configured to receive one or more reactants through the inlet port and to allow the reactants to react under a selected temperature and pressure and to produce one or more products exiting through the outlet port.

2. The microreactor of claim 1 wherein the brazing alloy permanently bonds the tubular heater with the metal capillary reaction tubing by first painting the brazing alloy over the metal capillary reaction tubing and the outer heater sheath and then reflowing the brazing alloy by raising the temperature of the microreactor above the brazing alloy's melting temperature and subsequently solidifying the reflowed brazing alloy by reducing the temperature of the microreactor below the brazing alloy's melting temperature.

3. The microreactor of claim 1 , wherein the brazing alloy comprises a silver-nickel brazing alloy paste or a silver solder.

4. The microreactor of claim 1 , wherein the metal capillary reaction tubing comprises a nickel electroformed tubing or stainless steel tubing.

5. The microreactor of claim 4 , wherein the metal capillary reaction tubing comprises a coated inner surface.

6. The microreactor of claim 4 , wherein the inner surface of the metal capillary reaction tubing is coated with silica.

7. The microreactor of claim 4 , wherein the inner surface of the metal capillary reaction tubing is coated with silica via atomic layer deposition or chemical vapor deposition after it is installed into the microreactor.

8. The microreactor of claim 1 , further comprising a cooling line being wrapped around the tubular heater and arranged parallel to the metal capillary reaction tubing.

9. The microreactor of claim 1 , further comprising an outer insulating layer.

10. The microreactor of claim 1 , further comprising a high surface area support uniformly deposited in the inner wall of the metal capillary reaction tubing.

11. The microreactor of claim 10 , wherein the high surface area support comprises an aerogel deposited in-situ in the inner wall of the metal capillary reaction tubing.

12. The microreactor of claim 11 , wherein the aerogel is uniformly deposited in the inner wall of the metal capillary reaction tubing by first flowing a solution comprising a pre-methanolyzed or partially methanolyzed solution of nitric acid, urea, water, and tetramethyl orthosilicate (TMOS) through the metal capillary reaction tubing, next heating the microreactor to break down the urea and to produce ammonium hydroxide, subsequently neutralizing the nitric acid with the ammonium hydroxide to produce ammonium nitrate and to produce a basic solution, next increasing the reaction rate of condensation with the basic solution thereby resulting in a polymer-like gel of amorphous silica and finally removing residual byproducts via supercritical drying thereby resulting in a uniformly deposited silica aerogel.

13. The microreactor of claim 12 , further comprising a small open channel through the center of the deposited aerogel and wherein said open channel reduces the pressure drop across the microreactor, and provides reactant and product exchange with the aerogel via diffusion.

14. The microreactor of claim 13 , wherein the open channel is formed by threading a narrow carbon filament through the metal capillary reaction tubing and then burning the carbon filament out after the aerogel is deposited.

15. A microreactor system comprising a plurality of cartridge microreactors connected with each other in series and wherein each cartridge microreactor comprises:

a tubular heater comprising an inner tube surrounded by an outer heater sheath;

a metal capillary reaction tubing comprising an inlet port and an outlet port and being wrapped around the tubular heater so that it is in intimate thermal contact with the heater sheath; and

a brazing alloy permanently bonding the tubular heater with the metal capillary reaction tubing; and

wherein the metal capillary reaction tubing is configured to be heated by the tubular heater and is configured to receive one or more reactants through the inlet port and to allow the reactants to react under a selected temperature and pressure and to produce one or more products exiting through the outlet port.

16. A microreactor system comprising a plurality of cartridge microreactors connected with each other in parallel and wherein each cartridge microreactor comprises:

a tubular heater comprising an inner tube surrounded by an outer heater sheath;

a metal capillary reaction tubing comprising an inlet port and an outlet port and being wrapped around the tubular heater so that it is in intimate thermal contact with the heater sheath; and

a brazing alloy permanently bonding the tubular heater with the metal capillary reaction tubing; and

wherein the metal capillary reaction tubing is configured to be heated by the tubular heater and is configured to receive one or more reactants through the inlet port and to allow the reactants to react under a selected temperature and pressure and to produce one or more products exiting through the outlet port.

17. A method for producing a cartridge microreactor comprising:

providing a tubular heater comprising an inner tube surrounded by an outer heater sheath;

providing a metal capillary reaction tubing comprising an inlet port and an outlet port and wrapping the metal capillary reaction tubing around the tubular heater so that it is in intimate thermal contact with the heater sheath; and

permanently bonding the tubular heater with the metal capillary reaction tubing with a brazing alloy; and

wherein the metal capillary reaction tubing is configured to be heated by the tubular heater and is configured to receive one or more reactants through the inlet port and to allow the reactants to react under a selected temperature and pressure and to produce one or more products exiting through the outlet port.

18. The method of claim 17 , wherein the tubular heater is permanently bonded with the metal capillary reaction tubing by first painting the brazing alloy over the metal capillary reaction tubing and the outer heater sheath and then reflowing the brazing alloy by raising the temperature of the microreactor above the brazing alloy's melting temperature and subsequently solidifying the reflowed brazing alloy by reducing the temperature of the microreactor below the brazing alloy's melting temperature.

19. The method of claim 17 , wherein the brazing alloy comprises a silver-nickel brazing alloy paste or a silver solder.

20. The method of claim 17 , wherein the metal capillary reaction tubing comprises a nickel electroformed tubing or stainless steel tubing.

21. The method of claim 20 , wherein the metal capillary reaction tubing comprises a coated inner surface.

22. The method of claim 21 , wherein the inner surface of the metal capillary reaction tubing is coated with silica.

23. The method of claim 21 , wherein the inner surface of the metal capillary reaction tubing is coated with silica via atomic layer deposition or chemical vapor deposition after it is installed into the microreactor.

24. The method of claim 17 , further comprising providing a cooling line and wrapping the cooling line around the tubular heater so that it is parallel to the metal capillary reaction tubing.

25. The method of claim 17 , further comprising providing an outer insulating layer and insulating the microreactor.

26. The method of claim 17 , further comprising depositing a high surface area support uniformly in the inner wall of the metal capillary reaction tubing and wherein the high surface area support comprises an aerogel.

27. The method of claim 26 , wherein the aerogel is uniformly deposited in the inner wall of the metal capillary reaction tubing by first flowing a solution comprising a pre-methanolyzed or partially methanolyzed solution of nitric acid, urea, water, and tetramethyl orthosilicate (TMOS) through the metal capillary reaction tubing, next heating the microreactor to break down the urea and to produce ammonium hydroxide, subsequently neutralizing the nitric acid with the ammonium hydroxide to produce ammonium nitrate and to produce a basic solution, next increasing the reaction rate of condensation with the basic solution thereby resulting in a polymer-like gel of amorphous silica and finally removing residual byproducts via supercritical drying thereby resulting in a uniformly deposited silica aerogel.

28. The method of claim 27 , further comprising forming a small open channel through the center of the deposited aerogel and wherein said open channel reduces the pressure drop across the microreactor, and provides reactant and product exchange with the aerogel via diffusion.

29. The method of claim 28 , wherein the open channel is formed by threading a narrow carbon filament through the metal capillary reaction tubing and then burning out the carbon filament after the aerogel is deposited.

30. The method of claim 28 further comprising depositing a catalyst on the high surface area support via atomic layer deposition.

Assignments (2)
CHANGE OF NAME Recorded Oct 1, 2014
From: MICROREACTOR SOLUTIONS LLC
To: NAVOLTA LLC
Reel/Frame 033859/0532 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 16, 2012
From: NELTNER, BRIAN; KING, DAVID M.; WOODRUF, RICK BRYAN
To: MICROREACTOR SOLUTIONS LLC
Reel/Frame 028557/0713 →
Continuity (2)
Provisional Application 61494548 · Jun 8, 2011
Related Publication 20120315199A1 · Dec 13, 2012