Apparatus and methods for parallel processing of multiple reaction mixtures

Abstract

An apparatus for parallel processing of multiple reaction mixtures comprises a plurality of reactor vessels for holding reaction mixtures at pressures of at least about 15 psig. Cannula passages communicate with respective vessels, and a cannula is adapted to be inserted into each cannula passage. A sealing mechanism, comprising a valve and a seal, in each cannula passage maintains a respective vessel sealed when the cannula is inserted into and withdrawn from the cannula passage. A robot system is operable to insert the cannula to a location where a distal end and port of the cannula are past the open valve and seal, and to withdraw the cannula. Methods for transferring fluid reaction material to and from a series of pressurized vessels, establishing fluid communication between a cannula and a vessel of a combinatorial chemistry reactor and establishing fluid communication between a cannula and a series of pressurized vessels of a combinatorial chemistry reactor are also disclosed.

What is claimed is:  
     
         1 . Apparatus for parallel processing of multiple reaction mixtures, said apparatus comprising 
 a plurality of reactor vessels for holding said reaction mixtures at pressures of at least about 15 psig,    cannula passages communicating with respective vessels,    a cannula adapted to be inserted into each cannula passage, said cannula having a distal end and a port generally adjacent said distal end,    a sealing mechanism in each cannula passage for maintaining a respective vessel sealed at said pressure of at least 15 psig when the cannula is inserted into and withdrawn from the cannula passage, said sealing mechanism comprising a valve movable between a normally closed position and an open position permitting movement of the cannula through the cannula passage past the valve, and a seal adapted for sealing contact with the cannula when the valve is in its open position, and    a robot system operable to insert the cannula through a selected cannula passage to a fluid transfer location, and to withdraw the cannula from the selected cannula passage.    
     
     
         2 . Apparatus as set forth in  claim 1  wherein said pressures are up to about 500 psig.  
     
     
         3 . Apparatus as set forth in  claim 1  wherein said pressures are at least about 50-100 psig.  
     
     
         4 . Apparatus as set forth in  claim 1  wherein said valve has a body and a central passage through the body forming part of the cannula passage.  
     
     
         5 . Apparatus as set forth in  claim 4  wherein said valve comprises a duckbill valve comprising duckbill lips formed integrally with the body.  
     
     
         6 . Apparatus as set forth in  claim 5  further comprising a spring which biases the lips together to close the central passage.  
     
     
         7 . Apparatus as set forth in  claim 5  wherein said lips of the duckbill valve close after the cannula is pulled past the lips during said withdrawal.  
     
     
         8 . Apparatus as set forth in  claim 1  wherein said seal is located on a side of the valve opposite the vessel.  
     
     
         9 . Apparatus as set forth in  claim 8  wherein said seal is spaced from said valve.  
     
     
         10 . Apparatus as set forth in  claim 9  wherein said robot system is operable to insert said cannula to said fluid transfer location in which the distal end of the cannula is downstream from the valve for fluid communication between said port and a respective vessel, then to withdraw the cannula to a dwell position in which the distal end of the cannula is between the valve and said seal, the robot system holding the cannula in said dwell position for a period sufficient to allow the valve to close prior to completely withdrawing the cannula from the cannula passage.  
     
     
         11 . Apparatus as set forth in  claim 1  wherein said robot system is operable to insert said cannula to said fluid transfer location for effecting the transfer of fluid materials to a respective vessel.  
     
     
         12 . Apparatus as set forth in  claim 1  wherein said robot system is operable to insert said cannula to said fluid transfer location for effecting the transfer of fluid materials from a respective vessel.  
     
     
         13 . Apparatus as set forth in  claim 1  further comprising a reactor block containing said vessels, said cannula passages extending in the reactor block between respective vessels and an exterior surface of the reactor block.  
     
     
         14 . Apparatus as set forth in  claim 1  further comprising a wiper adjacent an inlet end of each cannula passage for wiping the exterior surface of the cannula as it is inserted in the passage to wipe away any material thereon.  
     
     
         15 . Apparatus as set forth in  claim 1  wherein said cannula comprises a long metal tube, and wherein said apparatus further comprises a cannula support on the robot engageable with the tube intermediate the ends of the tube for supporting and stabilizing the tube in precise position as the cannula is moved.  
     
     
         16 . Apparatus as set forth in  claim 15  wherein said cannula support comprises a body affixed to the cannula mount and a head mounted on the body and having an opening therein sized for a close clearance fit with said long metal tube, said head being movable relative to the body from an extended position in which the head is spaced from the body for engagement with a more distal portion of the tube, and a retracted position in which the head is closer to the body for engagement with a more proximal portion of the tube to allow for insertion of the said more distal portion of the tube into a cannula passage.  
     
     
         17 . Apparatus as set forth in  claim 1  wherein said cannula comprises a reservoir for holding a volume of said reaction material, said reservoir having an outside diameter, and a long thin tubular needle in fluid communication with said reservoir and having an outside diameter less than the outside diameter of the reservoir.  
     
     
         18 . Apparatus as set forth in  claim 1  further comprising a heated wash tower having a well therein for receiving a portion of a cannula to be cleaned, said tower having a heater for heating fluid in the well to clean said portion of the cannula.  
     
     
         19 . Apparatus as set forth in  claim 1  wherein said valve moves to said closed position in response to withdrawal of the cannula from said passage.  
     
     
         20 . A method of transferring fluid reaction material into a series of pressurized vessels, said method comprising: 
 (1) inserting a cannula into a cannula passage communicating with a respective vessel pressurized to at least about 15 psig, said inserting comprising moving the cannula in the cannula passage through a normally closed valve in the passage to a fluid transfer location where the distal end of the cannula is past the valve and a seal is in sealing contact with the cannula to prevent substantial leakage from the pressurized vessel,    (2) transferring a fluid reaction material from said cannula into the vessel pressurized to at least about 15 psig,    (3) withdrawing the cannula from said passage, and    (4) repeating 1-3 for a second vessel.    
     
     
         21 . A method as set forth in  claim 20  wherein said vessels are at pressures of up to about 500 psig.  
     
     
         22 . Apparatus as set forth in  claim 20  wherein said vessels are at pressures of at least about 50-100 psig.  
     
     
         23 . A method as set forth in  claim 20  wherein said cannula has an outside surface, and wherein said method further comprises wiping the outside surface as the cannula is inserted in said cannula passage.  
     
     
         24 . A method as set forth in  claim 20  wherein said seal is spaced from said valve.  
     
     
         25 . A method as set forth in  claim 24  wherein said seal is located on a side of the valve opposite said vessel, and wherein said withdrawing comprises withdrawing the cannula to a dwell position in which the distal end of the cannula is located between the valve and said seal, and holding the cannula in said dwell position for a period sufficient to allow the valve to close before completely withdrawing the cannula from the cannula passage.  
     
     
         26 . A method as set forth in  claim 20  wherein said reaction material is a slurry comprising a catalyst fluid.  
     
     
         27 . A method as set forth in  claim 26  wherein said catalyst is disposed on a particulate support.  
     
     
         28 . A method as set forth in  claim 20  further comprising cleaning the cannula after withdrawing it from said cannula passage, said cleaning comprising washing and rinsing the cannula using a heated solution.  
     
     
         29 . A method as set forth in  claim 20  further comprising cleaning the cannula after withdrawing it from said cannula passage, said cleaning comprising subjecting said cannula to ultrasonic waves.  
     
     
         30 . A method as set forth in  claim 20  wherein said valve is spring-biased toward a normally closed position, and wherein said cannula forces the valve open as the cannula is moved through the passage.  
     
     
         31 . A method as set forth in  claim 20  wherein said fluid transfer location is one where the distal end of the cannula is in said vessel.  
     
     
         32 . A method of transferring fluid reaction material from a series of pressurized vessels, said method comprising: 
 (1) inserting a cannula into a cannula passage communicating with a respective vessel pressurized to at least about 15 psig, said inserting comprising moving the cannula in the cannula passage through a normally closed valve in the passage to a fluid transfer location where the distal end of the cannula is past the valve and a seal is in sealing contact with the cannula to prevent substantial leakage from the pressurized vessel,    (2) transferring a fluid reaction material to said cannula from the vessel pressurized to at least about 15 psig,    (3) withdrawing the cannula from said passage, and    (4) repeating 1-3 for a second vessel.    
     
     
         33 . A method as set forth in  claim 32  wherein said vessels are at pressures of up to about 500 psig.  
     
     
         34 . A method as set forth in  claim 32  wherein said vessels are at pressures of at least about 50-100 psig.  
     
     
         35 . A method as set forth in  claim 32  wherein said cannula has an outside surface, and wherein said method further comprises wiping the outside surface as the cannula is inserted in said cannula passage.  
     
     
         36 . A method as set forth in  claim 32  wherein said seal is spaced from said valve.  
     
     
         37 . A method as set forth in  claim 36  wherein said seal is located on a side of the valve opposite said vessel, and wherein said withdrawing comprises withdrawing the cannula to a dwell position in which the distal end of the cannula is located between the valve and said seal, and holding the cannula in said dwell position for a period sufficient to allow the valve to close before completely withdrawing the cannula from the cannula passage.  
     
     
         38 . A method as set forth in  claim 32  wherein said valve is spring-biased toward a normally closed position, and wherein said cannula forces the valve open as the cannula is moved through the passage.  
     
     
         39 . A method as set forth in  claim 32  wherein said fluid transfer location is one where the distal end of the cannula is in said vessel.