Apparatus and methods for parallel processing of multiple...

Chemical apparatus and process disinfecting – deodorizing – preser – Chemical reactor – Bench scale

Reexamination Certificate

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C422S129000, C422S131000, C422S198000, C422S224000, C422S225000, C422S226000, C422S232000, C436S037000, C436S155000, C436S159000

Reexamination Certificate

active

06759014

ABSTRACT:

BACKGROUND OF THE INVENTION
The present invention relates generally to parallel reactors, and in particular, to parallel research reactors suitable for use in a combinatorial (i.e., high-throughput) science research program in which chemical reactions are conducted simultaneously using small volumes of reaction materials to efficiently and economically screen large libraries of chemical materials.
SUMMARY OF THE INVENTION
In view of the foregoing, the objectives of this invention include the provision of a parallel reactor and related methods which overcome deficiencies of known parallel reactors, especially parallel research reactors and methods; the provision of such a parallel reactor and methods which allow for the efficient handling of slurry reactant materials, including slurries containing small particles of solid material, such as silica, and slurries which are especially “sticky” and thus difficult to handle; the provision of such a reactor and methods which provide for the delivery of precise quantities of reactant products, including slurries, to the reaction vessels of a parallel reactor; and the provision of such a reactor and methods which provide for the delivery of slurry and other reaction materials under pressure and/or temperature to one or more reaction chambers of the reactor.
In general, apparatus of the present invention is operable for processing multiple reaction mixtures in parallel. In one aspect, the apparatus comprises a reactor having an exterior surface, and vessels in the reactor for holding the reaction mixtures, each vessel having a central longitudinal axis. A cannula is used for introducing fluid reaction material into the vessels. The cannula has a longitudinal axis, a distal end, and a port generally adjacent said distal end for delivery of reaction material from the cannula. Cannula passages in the reactor extend between the exterior surface of the reactor and the vessels. Each passage extends at an angle relative to the central longitudinal axis of a respective vessel. A robot system is operable to insert the cannula through a selected cannula passage and into a respective vessel for the delivery of the reaction material from the cannula to the respective vessel, and to withdraw the cannula from the selected cannula passage and respective vessel.
Another aspect of the present invention involves a method of loading fluid reaction material into a series of vessels in a reactor, each vessel having a central longitudinal axis. The method comprises, in sequence, (1) inserting a cannula through a cannula passage in the reactor to a position in which the cannula extends at an angle relative to the central longitudinal axis of a first vessel of the series of vessels, and in which a distal end of the cannula is disposed in the vessel, (2) delivering a fluid reaction material from the cannula into the vessel, (3) withdrawing the cannula from said passage, and repeating 1-3 for a second vessel.
The present invention is also directed to a cannula for use in aspirating reactant materials and delivering such materials to reaction vessels for the parallel processing of such materials. The cannula comprises a tubular metal reservoir having a longitudinal axis, an inside diameter defining a hollow interior for containing said reactant materials, an outside diameter, a proximal end and a distal end. The cannula also includes a long straight thin needle formed from metal tubing and coaxial with the reservoir. The needle has an outside diameter substantially less than the outside diameter of the reservoir and an inside diameter defining a flow passage through the needle. The needle further has a proximal end, a distal end, and a port adjacent the distal end for aspirating reactant materials into the needle and delivering reactant materials from the needle. A metal transition joins the proximal end of the needle to the distal end of the reservoir so that the hollow of the interior of the reservoir is in fluid communication with the flow passage of the needle.
Another aspect of the present invention involves vessels designed for placement in a series of vertical cylindric wells in a parallel reactor of the type having cannula passages extending at an angle off vertical from an exterior surface of the reactor to the wells, each cannula passage being adapted for the passage therethrough of a cannula containing reaction material to be delivered to a respective vessel. Each vessel has a bottom and a cylindric side wall extending up from the bottom and terminating in a rim defining an open upper end of the vessel. The cylindric side wall has an inside diameter in the range of 0.5-2.5 in. The vessel has a volume in the range of 5-200 ml. and an overall height in the range of 1.0-4.0 in., such that when the vessel is placed in a well of the reactor, the open upper end of the vessel is disposed at an elevation below the cannula passage where the cannula passage enters the well and is positioned for entry of the cannula down through the open upper end of the vessel to a position below the rim of the vessel for the delivery of reactant materials into the vessel.
In yet another aspect, the present invention involves a method of preparing and delivering a slurry reaction material into a series of vessels in a reactor. The method comprises (1) mixing a particulate solid material and a liquid to form a substantially homogeneous first slurry in which the particulate solid material is suspended in the liquid, (2) aspirating the first slurry into a cannula carried by a robot system while the slurry is substantially homogeneous, (3) operating the robot system to insert the cannula into the reactor, (4) delivering the slurry from the cannula into the vessel while the cannula is in said cannula passage, and (5) repeating 2-4 for a second vessel and optionally a second slurry.
Other objects and features will be in part apparent and in part pointed out hereinafter.


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